THIRD SUPPLEMENT TO THE FOURTH EDITION
FOOD CHEMICALS CODEX Effective December 31, 2001
NATIONAL ACADEMY PRESS Washin...
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THIRD SUPPLEMENT TO THE FOURTH EDITION
FOOD CHEMICALS CODEX Effective December 31, 2001
NATIONAL ACADEMY PRESS Washington, D.C.
NATIONAL ACADEMY PRESS
• 2101 Constitution Avenue, N.W.
•
Washington, DC 20418
NOTICE: The project that is the subject of this report was approved by the Governing Board of the National Research Council, whose members are drawn from the councils of the National Academy of Sciences, the National Academy of Engineering, and the Institute of Medicine. The members of the committee responsible for the report were chosen for their special competences and with regard for appropriate balance. Support for this project was provided by U.S. Food and Drug Administration Contract No. 223-99-2321. The views presented in this report are those of the Institute of Medicine Committee on Food Chemicals Codex and are not necessarily those of the funding agencies. International Standard Book Number 0-309-07430-4 Library of Congress Control Number: 2001096469 Additional copies of this report are available for sale from the National Academy Press, 2101 Constitution Avenue, N.W., Box 285, Washington, D.C. 20055. Call (800) 624-6242 or (202) 334-3313 (in the Washington metropolitan area), or visit the NAP’s home page at www.nap.edu. The index of this report is available at www.nap.edu. For more information about the Institute of Medicine, visit the IOM home page at: www.iom.edu. Copyright 2001 by the National Academy of Sciences. All rights reserved. Printed in the United States of America. The serpent has been a symbol of long life, healing, and knowledge among almost all cultures and religions since the beginning of recorded history. The serpent adopted as a logotype by the Institute of Medicine is a relief carving from ancient Greece, now held by the Staatliche Museen in Berlin.
“Knowing is not enough; we must apply. Willing is not enough; we must do.” —Goethe
INSTITUTE OF MEDICINE Shaping the Future for Health
National Academy of Sciences National Academy of Engineering Institute of Medicine National Research Council
The National Academy of Sciences is a private, nonprofit, self-perpetuating society of distinguished scholars engaged in scientific and engineering research, dedicated to the furtherance of science and technology and to their use for the general welfare. Upon the authority of the charter granted to it by the Congress in 1863, the Academy has a mandate that requires it to advise the federal government on scientific and technical matters. Dr. Bruce M. Alberts is president of the National Academy of Sciences. The National Academy of Engineering was established in 1964, under the charter of the National Academy of Sciences, as a parallel organization of outstanding engineers. It is autonomous in its administration and in the selection of its members, sharing with the National Academy of Sciences the responsibility for advising the federal government. The National Academy of Engineering also sponsors engineering programs aimed at meeting national needs, encourages education and research, and recognizes the superior achievements of engineers. Dr. Wm. A. Wulf is president of the National Academy of Engineering. The Institute of Medicine was established in 1970 by the National Academy of Sciences to secure the services of eminent members of appropriate professions in the examination of policy matters pertaining to the health of the public. The Institute acts under the responsibility given to the National Academy of Sciences by its congressional charter to be an adviser to the federal government and, upon its own initiative, to identify issues of medical care, research, and education. Dr. Kenneth I. Shine is president of the Institute of Medicine. The National Research Council was organized by the National Academy of Sciences in 1916 to associate the broad community of science and technology with the Academy’s purposes of furthering knowledge and advising the federal government. Functioning in accordance with general policies determined by the Academy, the Council has become the principal operating agency of both the National Academy of Sciences and the National Academy of Engineering in providing services to the government, the public, and the scientific and engineering communities. The Council is administered jointly by both Academies and the Institute of Medicine. Dr. Bruce M. Alberts and Dr. Wm. A. Wulf are chairman and vice chairman, respectively, of the National Research Council.
COMMITTEE ON FOOD CHEMICALS CODEX S. Suzanne Nielsen (Chair (2001– ); Vice-Chair (1998–2000), Department of Food Science, Purdue University, West Lafayette, Indiana Steve L. Taylor (Chair 1989–2000), Department of Food Science and Technology, Food Processing Center, University of Nebraska, Lincoln Michael H. Auerbach, Danisco Cultor America, Inc., Ardsley, New York Jonathan DeVries, General Mills, Inc., Minneapolis, Minnesota Mark Dreher, Mead Johnson Nutritionals, Evansville, Indiana E. Allen Foegeding (2000–2001), Department of Food Science, North Carolina State University, Raleigh Carl Frey, Givaudan, East Hanover, New Jersey David S. Frick, Warner Jenkinson Company, St. Louis, Missouri Glen Ishikawa, NutraSweet Company, Mt. Prospect, Illinois Richard W. Lane, Unilever Bestfoods NA, Englewood Cliffs, New Jersey Merle D. Pierson, Department of Food Science and Technology, Virginia Polytechnic Institute and State University, Blacksburg John W. Salminen, Health Canada, Ottawa, Ontario, Canada Shelly Schmidt, Department of Food Science and Human Nutrition, University of Illinois at Champaign-Urbana Pamela J. White, Food Science and Human Nutrition Department, Iowa State University, Ames Consultants Grady W. Chism, III, Department of Food Science and Technology, Ohio State University, Columbus Andrew G. Ebert, The Kellen Company, Atlanta, Georgia Staff Ricardo A. Molins, Project Director Marcia S. Lewis, Research Assistant FOOD AND NUTRITION BOARD Cutberto Garza (Chair), Department of Nutrition Sciences, Cornell University, Ithaca, New York Alfred H. Merrill, Jr. (Vice-Chair), Department of Biochemistry and Center for Nutrition and Health Sciences, Emory University, Atlanta, Georgia Robert M. Russell (Vice-Chair), USDA Human Nutrition Research Center on Aging, Tufts University, Boston, Massachusetts Virginia A. Stallings (Vice-Chair), Division of Gastroenterology and Nutrition, The Children’s Hospital of Philadelphia, Pennsylvania Larry R. Beuchat, Center for Food Safety and Quality Enhancement, University of Georgia, Griffin Benjamin Caballero, Center for Human Nutrition, Johns Hopkins School of Hygiene and Public Health, Baltimore, Maryland Robert J. Cousins, Center for Nutritional Sciences, University of Florida, Gainesville Shiriki Kumanyika, Center for Clinical Epidemiology and Biostatistics, University of Pennsylvania School of Medicine, Philadelphia Lynn Parker, Food Research and Action Center, Washington, D.C. Ross L. Prentice, Division of Public Health Sciences, Fred Hutchinson Cancer Research Center, Seattle, Washington A. Catharine Ross, Nutrition Department, Pennsylvania State University, University Park Barbara O. Schneeman, Department of Nutrition, University of California, Davis Robert E. Smith, R.E. Smith Consulting, Inc., Newport, Vermont Steve L. Taylor, Department of Food Science and Technology, Food Processing Center, University of Nebraska-Lincoln Barry L. Zoumas, Department of Agricultural Economics and Rural Sociology, Pennsylvania State University, University Park Staff Allison A. Yates, Director Linda Meyers, Deputy Director Gary Walker, Financial Associate
v
Reviewers
This report has been reviewed in draft form by individuals chosen for their diverse perspectives and technical expertise, in accordance with procedures approved by the NRC’s Report Review Committee. The purpose of this independent review is to provide candid and critical comments that will assist the institution in making its published report as sound as possible and to ensure that the report meets institutional standards for objectivity, evidence, and responsiveness to the study charge. The review comments and draft manuscript remain confidential to protect the integrity of the deliberative process. We wish to thank the following individuals for their review of this report: Francis P. Busta, University of Minnesota Ronald Eitenmiller, Cornell University Richard L. Hall, retired Earl G. Hammond, Iowa State University Although the reviewers listed above have provided many constructive comments and suggestions, they were not asked to endorse the conclusions or recommendations nor did they see the final draft of the report before its release. The review of this report was overseen by Joseph H. Hotchkiss, Cornell University, appointed by the Institute of Medicine, who was responsible for making certain that an independent examination of this report was carried out in accordance with institutional procedures and that all review comments were carefully considered. Responsibility for the final content of this report rests entirely with the authoring committee and the institution.
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The Third Supplement to the Fourth Edition of the Food Chemicals Codex contains additions and changes to certain sections of the original text and the First and Second Supplements. The Supplement contains each new or revised monograph in its entirety, each preceded by a boxed explanatory section. The exception is Section 3/Flavor Chemicals, in which the boxed sections follow each entry. The revised monographs supersede those in the Fourth Edition and its First and Second Supplements. However, changes in Section 5/General Tests and Assays (Appendixes I through X) of the Fourth Edition are specific to the relevant individual test or assay. The entire appendix in which the revised test or assay appears is not reprinted and it is necessary to still refer to the Fourth Edition for unchanged portions. Users of this Supplement are reminded to consult the general policies and guidelines given in Section 1/General Provisions and Requirements Applying to Specifications, Tests, and Assays of the Food Chemicals Codex, Fourth Edition, pages 1 through 7. The policies and guidelines given therein remain in effect and are pertinent to this supplement.
Contents Section
1
GENERAL PROVISIONS AND REQUIREMENTS APPLYING TO SPECIFICATIONS, TESTS, AND ASSAYS OF THE FOOD CHEMICALS CODEX … 1 Heavy Metals Limits Policy (revised) … 1
2
MONOGRAPH SPECIFICATIONS … 3 Acidified Sodium Chlorite Solutions (new) … 3 Ammonium Phosphate, Dibasic (revised) … 4 Ammonium Phosphate, Monobasic (revised) … 4 L-Arginine (revised) … 5 Aspartame–Acesulfame Salt (new) … 5 DL-Aspartic Acid (revised) … 7 L-Aspartic Acid (revised) … 7 Canola Oil (revised) … 8 Carmine (revised) … 10 Cellulose Gum (revised) … 11 Citric Acid (revised) … 12 Cocoa Butter Substitute (revised) … 13 Curdlan (new) … 15 gamma-Cyclodextrin (new) … 16 Enzyme Preparations (revised) … 17 Ethoxyquin (revised) … 23 FD&C Blue No. 1 (revised) … 24 FD&C Blue No. 2 (revised) … 24 vii
FD&C Green No. 3 (revised) … 25 FD&C Red No. 3 (revised) … 26 FD&C Red No. 40 (revised) … 27 FD&C Yellow No. 5 (revised) … 28 FD&C Yellow No. 6 (revised) … 29 Grape Skin Extract (revised) … 29 DL-Isoleucine (revised) … 30 L-Isoleucine (revised) … 31 Lanolin, Anhydrous (revised) … 31 Lemongrass Oil (revised) … 32 DL-Leucine (revised) … 32 Lovage Oil (revised) … 33 Maltitol (revised) … 33 Mentha Arvensis Oil, Partially Dementholized (revised) … 34 Pectins (revised) … 35 Polyglycerol Polyricinoleic Acid (new) … 38 Pork Collagen (new) … 39 Potassium Phosphate, Monobasic (revised) … 40 Potassium Phosphate, Tribasic (revised) … 41 Potassium Pyrophosphate (revised) … 41 Potassium Sorbate (revised) … 42 Potassium Tripolyphosphate (revised) … 43 L-Proline (revised) … 43 Quinine Hydrochloride (revised) … 44 Rapeseed Oil, Fully Hydrogenated (revised) … 44 Rapeseed Oil, Superglycerinated (revised) … 45 Salatrim (new) … 46 DL-Serine (revised) … 50 L-Serine (revised) … 50 Silicon Dioxide (revised) … 51 Sodium Acid Pyrophosphate (revised) … 52 Sodium Metaphosphate, Insoluble (revised) … 52 Sodium Phosphate, Dibasic (revised) … 53 Sodium Phosphate, Monobasic (revised) … 54 Sodium Phosphate, Tribasic (revised) … 54 Sodium Polyphosphates, Glassy (revised) … 55 Sodium Potassium Tripolyphosphate (revised) … 56 Sodium Trimetaphosphate (revised) … 56 Sodium Tripolyphosphate (revised) … 57 Solin Oil (new) … 58 Sorbic Acid (revised) … 59 Soy Protein Concentrate (new) … 59 Sucrose Acetate Isobutyrate (new) … 60 L-Threonine (revised) … 60 Triacetin (revised) … 61 L-Valine (revised) … 62
viii
3
FLAVOR CHEMICALS … 63 Acetaldehyde Diethyl Acetal (new) … 64 Acetoin (revised) … 64 2-Acetylpyrrole (revised) … 64 2-Acetyl Thiazole (new) … 64 Allyl Isothiocyanate (revised) … 64 Allyl Phenoxy Acetate (new) … 64 Allyl Propionate (new) … 66 1-Amyl Alcohol (revised) … 66 Amyl Butyrate (revised) … 66 Amyl Formate (revised) … 66 Borneol (new) … 66 2-sec-Butyl Cyclohexanone (new) … 66 Butyl 2-Methyl Butyrate (new) … 66 Butyric Acid (revised) … 66 Cinnamic Acid (revised) … 66 Cyclohexyl Acetate (revised) … 68 p-Cymene (revised) … 68 (E),(E)-2,4-Decadienal (revised) … 68 (E)-2-Decenal (revised) … 68 (Z)-4-Decenal (revised) … 68 1,2-Di-[(1′-ethoxy)ethoxy]propane (revised) … 68 Dihydrocarveol (revised) … 68 d-Dihydrocarvone (revised) … 68 Dimethyl Benzyl Carbinyl Butyrate (revised) … 70 2,3-Dimethylpyrazine (revised) … 70 2,5-Dimethylpyrrole (revised) … 70 Dimethyl Succinate (revised) … 70 Dimethyl Sulfide (revised) … 70 Diphenyl Ether (new) … 70 δ-Dodecalactone (revised) … 70 (E)-2-Dodecen-1-al (revised) … 70 Ethone (revised) … 72 Ethyl Acetoacetate (revised) … 72 Ethyl Benzoyl Acetate (revised) … 72 Ethyl-(E)-2-butenoate (revised) … 72 Ethylene Brassylate (revised) … 72 2-Ethyl Hexanol (revised) … 72 Ethyl Lactate (revised) … 72 Ethyl Levulinate (revised) … 72 Ethyl 2-Methylbutyrate (revised) … 72 Ethyl 2-Methylpentanoate (revised) … 74 Ethyl 3-Methylthiopropionate (revised) … 74 Ethyl Salicylate (revised) … 74 Ethyl 10-Undecenoate (revised) … 74
ix
Ethyl Valerate (revised) … 74 Farnesol (revised) … 74 d-Fenchone (new) … 74 Fenchyl Alcohol (new) … 74 Furfuryl Alcohol (new) … 74 2-Furyl Methyl Ketone (new) … 74 Fusel Oil, Refined (revised) … 76 (E),(E)-2,4-Heptadienal (revised) … 76 Heptanal (revised) … 76 2-Heptanone (revised) … 76 (Z)-4-Hepten-1-al (revised) … 76 (E)-2-Hexen-1-al (revised) … 76 (Z)-3-Hexenyl Isovalerate (revised) … 76 (Z)-3-Hexenyl 2-Methylbutyrate (revised) … 76 Hexyl Alcohol (revised) … 76 Hexyl Isovalerate (revised) … 78 Hexyl 2-Methylbutyrate (revised) … 78 Isoamyl Alcohol (revised) … 78 Isoamyl Benzoate (revised) … 78 Isoamyl Butyrate (revised) … 78 Isoamyl Phenyl Acetate (revised) … 78 Isoamyl Salicylate (revised) … 78 Isobutyl Cinnamate (revised) … 78 Isobutyraldehyde (revised) … 78 Isopropyl Acetate (revised) … 80 Levulinic Acid (revised) … 80 l-Limonene (revised) … 80 Menthol (revised) … 80 l-Menthone (revised) … 80 dl-Menthyl Acetate (revised) … 80 l-Menthyl Acetate (revised) … 80 2-Methoxy-3(5)-methylpyrazine (revised) … 82 2-Methyl Butanal (revised) … 82 3-Methyl Butanal (revised) … 82 2-Methylbutyl Acetate (revised) … 82 2-Methylbutyl Isovalerate (revised) … 82 Methyl Butyrate (revised) … 82 2-Methylbutyric Acid (revised) … 82 Methyl Ionones (revised) … 82 Methyl Isobutyrate (revised) … 82 Methyl-3-methylthiopropionate (revised) … 82 4-Methyl-2-pentanone (revised) … 84 2-Methyl Propyl 3-Methyl Butyrate (revised) … 84 4-Methyl-5-thiazole Ethanol (revised) … 84 Nerolidol (revised) … 84 (E),(E)-2,4-Nonadienal (revised) … 84
x
(E),(Z)-2,6-Nonadienal (revised) … 84 (E),(Z)-2,6-Nonadienol (revised) … 84 Nonanoic Acid (revised) … 84 (E)-2-Nonenal (revised) … 84 (E)-2-Nonen-1-ol (revised) … 86 (Z)-6-Nonen-1-ol (revised) … 86 3-Octanol (revised) … 86 1-Octen-3-yl Acetate (revised) … 86 1-Octen-3-yl Butyrate (revised) … 86 α-Pinene (revised) … 86 Propenylguaethol (revised) … 86 Propyl Acetate (revised) … 86 Propyl Alcohol (revised) … 86 Propyl Propionate (revised) … 88 Terpinen-4-ol (revised) … 88 α-Terpineol (revised) … 88 Terpinyl Acetate (revised) … 88 Terpinyl Propionate (revised) … 88 2-Tridecenal (revised) … 88 Trimethylamine (revised) … 88 3,5,5-Trimethyl Hexanal (revised) … 88 2,3,5-Trimethylpyrazine (revised) … 90 1,3,5-Undecatriene (revised) … 90 (E)-2-Undecenol (revised) … 90 Veratraldehyde (revised) … 90 Zingerone (revised) … 90
4
INFRARED SPECTRA … 93 Acetaldehyde Diethyl Acetal (new) … 94 2-Acetyl Thiazole (new) … 94 Allyl Phenoxy Acetate (new) … 95 Allyl Propionate (new) … 95 Aspartame–Acesulfame Salt (new) … 96 Borneol (new) … 96 2-sec-Butyl Cyclohexanone (new) … 97 Butyl 2-Methyl Butyrate (new) … 97 gamma-Cyclodextrin (new) … 98 Diphenyl Ether (new) … 98 d-Fenchone (new) … 99 Fenchyl Alcohol (new) … 99 Furfuryl Alcohol (new) … 100 2-Furyl Methyl Ketone (new) … 100 Salatrim (new) … 101 Sucrose Acetate Isobutyrate (new) … 101
xi
5
GENERAL TESTS AND ASSAYS … 103 Fluoride Limit Test (Method IV) (Appendix IIIB) (revised) … 103 α-Acetolactatedecarboxylase Activity (Appendix V) (new) … 104 Aminopeptidase (Leucine) Activity (Appendix V) (new) … 105 Lipase (Microbial) Activity for Medium- and Long-Chain Fatty Acids (Appendix V) (new) … 105 Lysozyme Activity (Appendix V) (new) … 106 Peroxide Value (Appendix VII) (revised) … 108 Curcumin Content (Appendix VIII) (revised) … 109 Solutions and Indicators … 110 Acetic Acid TS, Strong (new) … 110 Nickel Standard Solution TS (new) … 110 Quimociac TS (revised) … 110 Sodium Hydroxide, 1 N (revised) … 110
Index … 111 Cumulative Index … 117
xii
1
Provisions and ⁄ General Requirements Applying to Specifications, Tests, and Assays of the Food Chemicals Codex
is not the largest source of lead exposure, it is a significant one. While ingestion of FCC substances does not represent the major source of dietary lead, it is desirable to lower the lead limits for all FCC substances, particularly for those substances consumed in high amounts. Therefore, the committee’s policy is to reduce lead and other heavy metals limits to the lowest extent feasible, especially given that more recent evidence shows deleterious neurobehavioral effects occurring in children exposed to lead at levels below those previously considered acceptable. In setting limits for lead and other heavy metals, the committee considers the amount of a food chemical consumed, the feasibility of manufacturing a product within these limits, and the availability of analytical methods to ensure compliance. The constraints of good manufacturing practice and the availability of reliable analytical methods are often limiting factors in setting lower limits for lead and other heavy metals. The committee regards as one of its goals the assurance of the safety of properly used food chemicals. This means that FCC specifications will respond to advances in knowledge about new manufacturing methods, analytical techniques, or toxicology and safety issues.
POLICIES AND GUIDELINES
Revision: Lead and Heavy Metals Limits (Policy) revised to remove the heavy metals (as Pb) specifications and to replace them with individual tests for relevant heavy metals. Heavy Metals Limits (Policy) The Committee on Food Chemicals Codex notes the importance of providing limits for individual heavy metals as required by the source and composition of individual food additives. Thus, it has decided to progressively remove from the monographs the general heavy metals (as lead) limits and test and, based on the current level and availability of scientific information and on the policy stated below, to replace them with limits and tests for specific heavy metals such as lead, cadmium, and mercury as may be relevant to each substance. The committee recognizes the desirability of lowering exposure to lead and other heavy metals, especially in the case of infants and children. Overall exposure to heavy metals in general, and to lead in particular, is a public health concern. Although diet
1
2
⁄ Monographs
requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Mercury Transfer 2.0 mL of the Sample Solution into a 50-mL beaker, add 10 mL of water, 1 mL of dilute sulfuric acid (1:5), and 1 mL of potassium permanganate solution (1:25), cover with a watch glass, boil for a few s, and cool. Use the resulting solution as the Sample Preparation as directed under the Mercury Limit Test, Appendix IIIB. pH Determine as directed under pH Determination, Appendix IIB. Sodium Chlorite (21 CFR 173.325; “Determination of Sodium Chlorite: 50 ppm to 1500 ppm,” Alcide Corporation) Sample For solutions containing 40 to 250 ppm, use a 100g sample; for those containing 250 to 500 ppm, use a 50-g sample; for those containing 500 to 1100 ppm, use a 20-g sample; for those containing 1100 to 1500 ppm, use a 15-g sample. Procedure Transfer the sample into a tared 250-mL Erlenmeyer flask, and record the weight to the nearest 0.1 mg. Add a magnetic stirring bar. Add approximately 2 g of potassium iodide, place the flask over a magnetic stirrer, and stir until the potassium iodide crystals dissolve (about 1 min). Add 1 mL of 6 N hydrochloric acid, and stir for 30 s. Under continuous stirring, titrate the liberated iodine with standardized 0.025 N sodium thiosulfate (Na2S2O3). When most of the brownish iodine color has faded, add 2 mL of starch indicator solution, and titrate to a clear endpoint, allowing adequate mixing time between additions of titrant near the endpoint. Record the volume of titrant, V, in mL. Calculation Calculate the amount of Sodium Chlorite, in ppm, by the equation
This is a new monograph:
Acidified Sodium Chlorite Solutions
DESCRIPTION Acidified Sodium Chlorite (ASC) Solutions occur as clear, colorless to pale yellow liquids. The ASC Solutions are equilibrium mixtures of sodium chlorite (NaClO2) and chlorous acid (HClO2). ASC Solutions are produced by lowering the pH of a sodium chlorite solution using a safe and suitable acid to achieve a pH within the range of 2.3 to 3.9 depending on the intended use. Functional Use in Foods Antimicrobial agent in processing water used to spray, dip, rinse, or store food before processing, to be followed by rinsing in potable water or by blanching, cooking, or canning; sanitizing hard surfaces; broad-spectrum bactericide, virucide, fungicide, and sporicide. REQUIREMENTS Lead Not more than 1 mg/kg. Mercury Not more than 1 mg/kg. pH Between 2.3 and 3.9. Note: The pH is chosen depending on the application; it controls the concentration of metastable chlorous acid, which rapidly breaks down into chlorine dioxide, chloride, and in some applications, chlorate.
ppm of Sodium Chlorite = (V × N × 90.44 × 1000)/(W × 4),
Caution: To minimize the evolution of hazardous chlorine dioxide gas, do not adjust the pH below 2.3. Sodium Chlorite application.
in which V is the volume, in mL, of titrant; N is the normality of the sodium thiosulfate titrant; 90.44 is the molecular weight of Sodium Chlorite; 1000 is a conversion factor from mg/g to ppm; W is the sample weight, in g; and 4 is the milliequivalents of sodium thiosulfate per milliequivalent of Sodium Chlorite.
Between 40 and 1200 ppm, depending on the
TESTS
Alternative Methods The concentration of Sodium Chlorite can be determined also using ion chromatography by following U.S. Environmental Protection
Lead A 1.0-mL portion of the sample solution, mixed with 5 mL of water and 11 mL of 2.7 N hydrochloric acid, meets the
3
4 / Ammonium Phosphate, Dibasic / Monographs
Agency Method 300.11 or amperometrically by following American Public Health Association Method 4500ClO2.2 Packaging and Storage Store Sodium Chlorite solutions in closed, opaque containers. Avoid exposure to sun or ultraviolet light because it will generate chlorine dioxide gas in the solution.
Revision: Fluoride test corrected; Heavy Metals (as Pb) specification and determination deleted. Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limits for this substance: Cadmium, not more than 2 mg/kg; Lead, not more than 4 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
Ammonium Phosphate, Dibasic Diammonium Phosphate (NH4)2HPO4
Formula wt 132.06
INS: 342(ii)
CAS: [7783-28-0]
FCC IV, Supplement 3
TESTS Assay Dissolve about 600 mg, accurately weighed, in 40 mL of water, and titrate to a pH of 4.6 with 0.1 N sulfuric acid. Each mL of 0.1 N sulfuric acid is equivalent to 13.21 mg of (NH4)2HPO4. Arsenic A solution of 1 g in 35 mL of water meets the requirements of the Arsenic Test, Appendix IIIB. Fluoride Determine on a 2-g sample as directed in Method IV under the Fluoride Limit Test, Appendix IIIB. Packaging and Storage
Store in tight containers.
Revision: Fluoride test corrected; Heavy Metals (as Pb) specification and determination deleted. Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limits for this substance: Cadmium, not more than 2 mg/kg; Lead, not more than 4 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
Ammonium Phosphate, Monobasic Monoammonium Phosphate
DESCRIPTION
NH4H2PO4
Formula wt 115.03
INS: 342(i)
CAS: [7722-76-1]
White crystals, crystalline powder, or granules. It is freely soluble in water. The pH of a 1:100 solution is between 7.6 and 8.2. Functional Use in Foods agent; yeast food.
Buffer; dough conditioner; leavening
REQUIREMENTS Identification A 1:20 solution gives positive tests for Ammonium and for Phosphate, Appendix IIIA. Assay Not less than 96.0% and not more than 102.0% of (NH4)2HPO4. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 10 mg/kg. Lead (See the note at the beginning of this monograph.)
DESCRIPTION White crystals, crystalline powder, or granules. It is freely soluble in water. The pH of a 1:100 solution is between 4.3 and 5.0. Functional Use in Foods agent; yeast food.
Buffer; dough conditioner; leavening
REQUIREMENTS Identification A 1:20 solution gives positive tests for Ammonium and for Phosphate, Appendix IIIA. Assay Not less than 96.0% and not more than 102.0% of NH4H2PO4. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 10 mg/kg. Lead (See the note at the beginning of this monograph.)
1Hautman,
Daniel P. and Munch, David J. “Method 300.1: Determination of inorganic anions in drinking water by ion chromatography, Revision 1.0.” U.S. Environmental Protection Agency, Office of Ground Water and Drinking Water. 1997. Online. Available: http://www.epa.gov/OGWDW/methods/ sourcalt.html [accessed July 26, 2000]. 2Franson, MA, ed. 1998. Standard methods 4500-ClO , am2 perometric method II. In: Standard Methods for the Examination of Water and Wastewater, 20th Ed. Baltimore, MD: APHA/ AWWA/WEF. Pp. 4-73–4-79.
TESTS Assay Dissolve about 500 mg, accurately weighed, in 50 mL of water, and titrate to a pH of 8.0 with 0.1 N sodium hydroxide. Each mL of 0.1 N sodium hydroxide is equivalent to 11.50 mg of NH4H2PO4. Arsenic A solution of 1 g in 35 mL of water meets the requirements of the Arsenic Test, Appendix IIIB.
FCC IV, Supplement 3
Monographs / Aspartame–Acesulfame Salt / 5
Fluoride Determine on a 2-g sample as directed in Method IV under the Fluoride Limit Test, Appendix IIIB. Packaging and Storage
Specific Rotation, Appendix IIB Determine in a solution containing 8 g of a previously dried sample in sufficient 6 N hydrochloric acid to make 100 mL.
Store in tight containers. Packaging and Storage containers.
Store in well-closed, light-resistant
Revision: Identification test corrected; Heavy Metals (as Pb) specification and determination deleted. This is a new monograph: L-Arginine
Aspartame–Acesulfame Salt
L-2-Amino-5-guanidinovaleric Acid
APM–Ace; [2-carboxy-β-(N-(b-methoxycarbonyl-2-phenyl)ethylcarbamoyl)]ethanaminium 6-methyl-4-oxo-1,2,3-oxathiazin-3ide-2,2-dioxide; L-Phenylalanine, L-α-aspartyl-2-methyl ester compound with 6-methyl-1,2,3-oxathiazin-4(3H)-one 2,2-dioxide (1:1)
NHCH2CH2CH2CCOOH C
NH
H NH2
NH2
C6H14N4O2
Formula wt 174.20 CAS: [74-79-3] CH2
DESCRIPTION
HOOCCH2CHCONHCHCOOCH3
White crystals or a white crystalline powder. It is soluble in water, but insoluble in ether and sparingly soluble in alcohol. It is strongly alkaline, and its water solutions absorb carbon dioxide from the air.
NH3
O
Functional Use in Foods
N SO2 O
Nutrient; dietary supplement. CH3
REQUIREMENTS Identification Heat 5 mL of a 1:1000 solution with 1 mL of triketohydrindene hydrate TS (ninhydrin TS). A reddish purple color appears. Assay Not less than 98.5% and not more than 101.5% of C6H14N4O2, calculated on the dried basis. Lead Not more than 10 mg/kg. Loss on Drying Not more than 1.0%. Residue on Ignition Not more than 0.2%. Specific Rotation [α]20° D : Between +26.0° and +27.9° after drying; or [α]25° D : Between +25.8° and +27.7° after drying. TESTS Assay Dissolve about 200 mg, accurately weighed, in 3 mL of formic acid and 50 mL of glacial acetic acid, add 2 drops of crystal violet TS, and titrate with 0.1 N perchloric acid to a green endpoint or until the blue color disappears completely. Each mL of 0.1 N perchloric acid is equivalent to 8.710 mg of C6H14N4O2. Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Loss on Drying, Appendix IIC Dry at 105° for 3 h. Residue on Ignition, Appendix IIC Ignite 1 g as directed in the general method.
C18H23O9N3S
Formula wt 457.46 CAS: [106372-55-8]
DESCRIPTION Aspartame–Acesulfame Salt occurs as a white, crystalline powder. It is sparingly soluble in water and slightly soluble in alcohol. Functional Use in Foods
Sweetener.
REQUIREMENTS Identification An infrared absorption spectrum of a potassium bromide dispersion of Aspartame–Acesulfame Salt exhibits maxima only at the same wavelengths as that of a typical spectrum as shown in the section on Infrared Spectra. Assay Not less than 63.0% and not more than 66.0% of aspartame, calculated on the dried basis. Not less than 34.0% and not more than 37.0% of acesulfame, calculated as acid formed on the dried basis. 5-Benzyl-3,6-dioxo-2-piperazineacetic Acid (DKP) Not more than 0.5%. Lead Not more than 1 mg/kg.
6 / Aspartame–Acesulfame Salt / Monographs
Loss on Drying Not more than 0.5%. Optical (Specific) Rotation [α]20° D : Between +14.5° and +16.5°, calculated on the dried basis. Other Related Impurities Not more than 1.0%. Potassium Not more than 0.5%.
FCC IV, Supplement 3
min, and the approximate retention time of aspartame is 11 min). Measure the peak area response of 5-benzyl-3,6-dioxo-2-piperazineacetic acid in each chromatogram. Calculation Calculate the percentage of 5-benzyl-3,6dioxo-2-piperazineacetic acid in the sample by the formula 1000 × (AUCS)/(ASWU),
TESTS Assay (Note: Use a combination pH-electrode for all titrations.) Accurately weigh between 0.100 and 0.150 g of sample, and dissolve it in 50 mL of ethanol. Perform the titration under a flow of nitrogen. Titrate with standardized 0.1 N tetrabutylammonium hydroxide in methanol or 2-propanol. Determine the volume of titrant needed to reach the first equivalence point (V1 mL) and the second equivalence point (V2 mL). Perform a blank titration with 50 mL of ethanol. Calculate the percentage of acesulfame and aspartame, respectively, taken by the formulas [(V1 – VB) × N × 163]/(10 × W), [(V2 – V1) × N × 294]/(10 × W), in which V1, V2, and VB are the number of mL of 0.1 N tetrabutylammonium hydroxide in methanol or 2-propanol used for the sample (first and second equivalence points) and the blank, respectively; N is the normality; W is the weight, in g, of sample taken; and 163 and 294 are the formula weights of acesulfame and aspartame, respectively. 5-Benzyl-3,6-dioxo-2-piperazineacetic Acid Mobile Phase Weigh 5.6 g of potassium phosphate, monobasic, into a 1-L flask, add 820 mL of water, and dissolve. Use phosphoric acid to adjust the pH to 4.3, add 180 mL of methanol, and mix. Filter through a 0.45-µm disk, and de-gas. Diluting Solvent Add 200 mL of methanol to 1800 mL of water, and mix. Standard Preparation Transfer about 25 mg of USP Reference Standard 5-Benzyl-3,6-dioxo-2-piperazineacetic Acid, accurately weighed, into a 100-mL volumetric flask. Add 10 mL of methanol, and dissolve. Dilute to volume with water, and mix. Pipet 15 mL of this solution into a 50-mL volumetric flask, dilute to volume with the Diluting Solvent, and mix. Use a freshly prepared solution. Sample Preparation Transfer about 50 mg of sample, accurately weighed, into a 10-mL volumetric flask. Dilute to volume with Diluting Solvent, and mix. Use a freshly prepared solution. Chromatographic System Use a suitable high-pressure liquid chromatograph equipped with a detector measuring at 210 nm and a 250- × 4.6-mm column packed with octadecyl silanized silica (10-µm Partisil ODS-3, or equivalent) and operated under isocratic conditions at 40°. The flow rate of the Mobile Phase is about 2 mL/min. System Suitability The area responses of three replicate injections of the Standard Preparation show a relative standard deviation of not more than 2.0%. Procedure Separately inject equal 20-µL portions of the Standard Preparation and the Sample Preparation into the chromatograph, and record the chromatograms (the approximate retention time of 5-benzyl-3,6-dioxo-2-piperazineacetic acid is 4
in which AU and AS are the peak area responses of 5-benzyl-3,6dioxo-2-piperazineacetic acid in the Sample Preparation and in the Standard Preparation, respectively; CS is the concentration, in mg/mL, of 5-benzyl-3,6-dioxo-2-piperazineacetic acid in the Standard Preparation; and WU is the weight, in mg, of sample taken for the Sample Preparation. Lead Determine as directed for Method II in the Atomic Absorption Spectrophotometric Graphite Furnace Method under the Lead Limit Test, Appendix IIIB. Loss on Drying Determine as directed under Loss on Drying, Appendix IIC, drying a sample at 105° for 4 h. Optical (Specific) Rotation Determine as directed under Optical (Specific) Rotation, Appendix IIB, using a solution containing 6.2 g of sample in sufficient 15 N formic acid to make 100 mL. Make the determination within 30 min of preparation of the sample solution. Divide the calculated specific rotation by 0.646 to correct for the Aspartame content in Aspartame–Acesulfame Salt. Other Related Impurities Proceed as directed in the test for 5Benzyl-3,6-dioxo-2-piperazineacetic Acid, but use the following Standard Preparation and Procedure: Standard Preparation Pipet 1.5 mL of the Sample Preparation from the test for 5-Benzyl-3,6-dioxo-2-piperazineacetic Acid into a 100-mL volumetric flask, dilute to volume with the Diluting Solvent, and mix. Procedure Separately inject equal 20-µL portions of the Standard Preparation and the Sample Preparation into the chromatograph, and record the chromatograms for a time equal to twice the retention time of Aspartame. In the chromatogram obtained from the Sample Preparation, the sum of the responses of all secondary peaks, other than that for 5-benzyl-3,6-dioxo-2piperazineacetic acid and Acesulfame, is not more than the response of the Aspartame peak obtained in the chromatogram from the Standard Preparation. Potassium Standard Solutions Transfer 190.7 mg of potassium chloride, previously dried at 105° for 2 h, to a 1000-mL volumetric flask, dilute with water to volume, and mix. Transfer 100.0 mL of this solution to a second 1000-mL volumetric flask, dilute with water to volume, and mix to obtain a Stock Solution containing 10 µg of potassium per mL (equivalent to 19.07 µg of potassium chloride). Into separate 100-mL volumetric flasks, pipet 10.0-, 15.0-, and 20.0-mL aliquots of the Stock Solution; add 2.0 mL of a 1:5 sodium chloride solution and 1.0 mL of hydrochloric acid to each; dilute with water to volume; and mix. The Standard Solutions obtained contain, respectively, 1.0, 1.5, and 2.0 µg of potassium per mL. Test Solution Transfer about 3.0 g of sample, accurately weighed, to a 500-mL volumetric flask, dilute with water, and mix. Transfer 10 mL of this solution to a 100-mL volumetric flask and add 2.0 mL of a 1:5 sodium chloride solution and 1.0 mL of
FCC IV, Supplement 3
Monographs / L-Aspartic Acid / 7
hydrochloric acid, dilute with water to volume, and mix. Filter the solution. Procedure Concomitantly determine the absorbances of the Standard Solutions and the Test Solution at the potassium emission line of 766.5 nm, with a suitable atomic absorption spectrophotometer equipped with a potassium hollow-cathode lamp and an air–acetylene flame, using water as the blank. Plot the absorbance of the Standard Solutions versus concentration, in µg/mL, of potassium, and draw the straight line best fitting the plotted points. From the graph so obtained, determine the concentration, C, in µg/mL, of potassium in the Test Solution. Calculate the percent potassium in the sample taken by the formula 500C/W,
green endpoint or until the blue color disappears completely. Perform a blank determination (see General Provisions), and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 13.31 mg of C4H7NO4. Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Loss on Drying, Appendix IIC Dry at 105° for 3 h. Residue on Ignition, Appendix IIC Ignite 1 g of sample as directed in the general method. Packaging and Storage containers.
Store in well-closed, light-resistant
in which W is the quantity, in mg, of sample taken to prepare the Test Solution. Packaging and Storage cool, dry place.
Store in well-closed containers in a
Revision: Identification test corrected; Heavy Metals (as Pb) specification and determination deleted. L-Aspartic Acid L-Aminosuccinic Acid
Revision: Identification test corrected; Heavy Metals (as Pb) specification and determination deleted.
HOOCCH2CCOOH H NH2
C4H7NO4
DL-Aspartic Acid
Formula wt 133.10 CAS: [56-84-8]
DL-Aminosuccinic Acid
HOOCCH2CH(NH2)COOH
C4H7NO4
Formula wt 133.11 CAS: [617-45-8]
DESCRIPTION White crystals or crystalline powder. It is slightly soluble in water, but insoluble in alcohol and in ether. It melts at about 270°. Functional Use in Foods
Nutrient; dietary supplement.
DESCRIPTION Colorless or white crystals. It is slightly soluble in water, but insoluble in alcohol and in ether. It is optically inactive and melts with decomposition at about 280°. Functional Use in Foods
Nutrient; dietary supplement.
REQUIREMENTS Identification Heat 5 mL of a 1:1000 solution with 1 mL of triketohydrindene hydrate TS (ninhydrin TS). A bluish purple color is produced. Assay Not less than 98.5% and not more than 101.5% of C4H7NO4, calculated on the dried basis. Lead Not more than 10 mg/kg. Loss on Drying Not more than 0.3%. Residue on Ignition Not more than 0.1%. TESTS Assay Dissolve about 200 mg of sample, accurately weighed, in 3 mL of formic acid and 50 mL of glacial acetic acid, add 2 drops of crystal violet TS, and titrate with 0.1 N perchloric acid to a
REQUIREMENTS Identification Heat 5 mL of a 1:1000 solution with 1 mL of triketohydrindene hydrate TS (ninhydrin TS). A bluish purple color appears. Assay Not less than 98.5% and not more than 101.5% of C4H7NO4, calculated on the dried basis. Lead Not more than 5 mg/kg. Loss on Drying Not more than 0.25%. Residue on Ignition Not more than 0.1%. Specific Rotation [α]D20°: Between +24.5° and +26.0° after drying. TESTS Assay Dissolve about 200 mg, accurately weighed, in 3 mL of formic acid and 50 mL of glacial acetic acid, add 2 drops of crystal violet TS, and titrate with 0.1 N perchloric acid to a green endpoint or until the blue color disappears completely. Perform a blank determination (see General Provisions), and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 13.31 mg of C4H7NO4.
8 / Canola Oil / Monographs
Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 5 µg of lead ion (Pb) in the control. Loss on Drying, Appendix IIC Dry at 105° for 3 h. Residue on Ignition, Appendix IIC Ignite 1 g of sample as directed in the general method. Specific Rotation, Appendix IIB Determine in a solution containing 8 g of a previously dried sample in sufficient 6 N hydrochloric acid to make 100 mL. Packaging and Storage containers.
Store in well-closed, light-resistant
Revision: Description and Functional Use in Foods modified, Heavy Metals (as Pb) specification and determination deleted.
Canola Oil Low Erucic Acid Rapeseed Oil; LEAR
DESCRIPTION Canola Oil occurs as a light yellow oil. It is typically obtained by a combination of mechanical expression followed by n-hexane extraction, from the seed of the plants Brassica juncea, Brassica napus, or Brassica rapa of the family Cruciferae. The plant varieties are those producing oil-bearing seeds with a low erucic acid (C22:1) content. It is a mixture of triglycerides composed of both saturated and unsaturated fatty acids. It is refined, bleached, and deodorized to substantially remove free fatty acids; phospholipids; color; odor and flavor components; and miscellaneous, other non-oil materials. It can be hydrogenated to reduce the level of unsaturated fatty acids for functional purposes in foods. It is a liquid at 0° and above. Functional Use in Foods Cooking or salad oil; component of margarine or shortening; coating agent; emulsifying agent; formulation aid; texturizer. REQUIREMENTS Labeling Hydrogenated Canola Oil less than fully hydrogenated must be labeled as Partially Hydrogenated Canola Oil. Identification Unhydrogenated Canola Oil exhibits the following composition profile of fatty acids as determined under Fatty Acid Composition, Appendix VII. Fatty Acid:
<14 14:0 16:0 16:1 18:0 18:1 18:2
Weight % (Range): <0.1 <0.2 <6.0 <1.0 <2.5 >50 <40.0 Fatty Acid:
18:3 20:0 20:1 22:0 22:1 24:0 24:1
Weight % (Range): <14 <1.0 <2.0 <0.5 <2.0 <0.2 <0.2 Acid Value Not more than 6.
FCC IV, Supplement 3
Cold Test Passes test. Color (AOCS-Wesson) Not more than 1.5 red/15 yellow. Erucic Acid Not more than 2.0%. Free Fatty Acids (as oleic acid) Not more than 0.05%. Iodine Value Between 110 and 126. Lead Not more than 0.1 mg/kg. Linolenic Acid Not more than 14.0%. Peroxide Value Not more than 10 meq/kg. Refractive Index Between 1.465 and 1.467 at 40°. Saponifiable Value Between 178 and 193. Stability Not less than 7 h. Sulfur Not more than 10 mg/kg. Unsaponifiable Matter Not more than 1.5%. Water Not more than 0.1%. TESTS Acid Value Determine as directed for Acid Value, Method II, under Fats and Related Substances, Appendix VII. Cold Test Proceed as directed under Cold Test, Appendix VII. Color Proceed as directed for Color (AOCS-Wesson) under Fats and Related Substances, Appendix VII. Use a 133.4-mm cell. Erucic Acid Determine as part of Fatty Acid Composition, Appendix VII. Free Fatty Acids Proceed as directed under Free Fatty Acids, Appendix VII, using the following equivalence factor (e) in the formula given in the procedure: Free fatty acids as oleic acid, e = 28.2. Iodine Value Proceed as directed under Modified Wijs Method, Appendix VII. Lead Determine as directed under Method II in the Atomic Absorption Spectrophotometric Graphite Furnace Method under the Lead Limit Test, Appendix IIIB, using a 1-g sample. Linolenic Acid Proceed as directed under Fatty Acid Composition, Appendix VII. Peroxide Value Proceed as directed under Peroxide Value in the monograph for Hydroxylated Lecithin. However, after the addition of saturated potassium iodide and mixing, mix the solution for only 1 min and begin the titration immediately instead of allowing the solution to stand for 10 min. Refractive Index, Appendix IIB Determine with an Abbé or other refractometer of equal or greater accuracy. Saponifiable Value Determine as directed under the general method, Appendix VII. Stability Proceed as directed under Stability, Appendix VII. Sulfur Organosulfur compounds present in the sample react with Raney nickel to produce nickel sulfides. Nickel sulfides are treated with a strong acid to produce hydrogen sulfide, which is trapped and titrated with mercuric acetate using a dithizone indicator. Caution: This test requires the use of the following hazardous substances: mercuric acetate, spongy nickel, and dibenzyl disulfide. Conduct the test in a fume hood. Apparatus Fit a 125-mL round-bottom boiling flask with a cylindrical filling funnel (20 mL with open top), an ST PTFE metering valve stopcock, and a gas inlet tube (see the figure for
FCC IV, Supplement 3
Raney Nickel Reduction Apparatus in Appendix IIIC under Sulfur (by Oxidative Microcoulometry). On top of the boiling flask, fit a water-jacketed distillation column with hooks. To the distillation column, fit a piece of glass tubing with ground ST inner joints with hooks, and connect the distillation column and a gas dispersion tube with ST outer joints with hooks. Dibenzyl Disulfide Solution Accurately weigh 0.75 g of dibenzyl disulfide and place in a 250-mL volumetric flask. Dilute to volume with methyl isobutyl ketone, and mix. Sulfur Standard Accurately weigh five 250.0-g samples of food-grade peanut oil. Transfer 0.0, 1.0, 2.0, 3.0, and 4.0 mL of the Dibenzyl Disulfide Solution into the peanut oil samples; the samples contain 0, 3, 6, 9, and 12 mg/kg of sulfur, respectively. Raney Nickel Preparation (Caution: Raney nickel is pyrophoric when dry.) Raney nickel is produced by reacting nickel– aluminum alloy with sodium hydroxide. Weigh accurately 1 g of nickel–aluminum alloy powder (50% Ni, 50% Al), place it in a 50-mL centrifuge tube, and chill it in an ice bath. Each pellet is enough catalyst for one determination. Slowly add 5 mL of water per tube, and let the tube stand for 10 min. Then, slowly add 10 mL of 2.5 N sodium hydroxide, and allow the mixture to react for 30 min. Cap the tubes, and place them in a 50° water bath for 2 h. Centrifuge the mixture at 1000 rpm for 10 min, and discard the supernatant liquid. Wash the pellets twice with 15 mL of water and twice with 15 mL of isopropanol, centrifuging between each wash. The catalyst may be stored under isopropanol for a period no longer than 2 weeks. Note: Properly dispose of the unused Raney Nickel Preparation by transferring it to a 250-mL Erlenmeyer flask, and placing it in a fume hood. Add 20 mL of 60% (w/v) hydrochloric acid, and allow complete digestion of the catalyst. Caution: Hydrogen gas evolves during the digestion process. Dithizone Indicator Solution Dissolve 10 mg of dithizone (diphenylthiocarbazone) in a 10-mL volumetric flask with acetone. Mercuric Acetate Titrant (Note: Mercuric acetate is a strong irritant when ingested or inhaled or upon dermal exposure.) Transfer 3.82 g of mercuric acetate into a 1000-mL volumetric flask containing 950 mL of water. Add 12.2 mL of glacial acetic acid, dilute to volume with water, and mix. Transfer 10.0 mL of this solution into a 100-mL volumetric flask, dilute to volume with water, and mix. The titrant solution contains 0.0012 M mercuric acetate. Titration Reagent Blank Add 50.0 mL of 1 N sodium hydroxide and 50.0 mL of acetone to a 250-mL beaker, and mix. Add 0.5 mL of the Dithizone Indicator Solution, and titrate with Mercuric Acetate Titrant until the color changes from bright amber to strawberry red. Record the volume of titrant used. Procedure Test a representative portion of the sample. Accurately weigh 15 to 20 g of the sample, and place it on the bottom of the boiling flask. Discard the isopropanol from the Raney Nickel Preparation, add 10 mL of 95% isopropanol, mix, and place the mixture in the sample oil. Attach the water condenser and the nitrogen line to the boiling flask and adjust the gas flow to 4 psi through the sample. Place a heating mantle under the
Monographs / Canola Oil / 9
flask. Immerse the bubbler in a 250-mL beaker containing 50.0 mL of 1 N sodium hydroxide, and stir slowly. Boil the sample for 90 min. Add 50 mL of acetone and 0.5 mL of Dithizone Indicator Solution to the 250-mL beaker. Add 20 mL of 60% hydrochloric acid into the filling funnel fitted onto the boiling flask, and adjust the nitrogen flow to 2 to 3 psi. Position the stir bar directly under the bubbler for maximum dispersion of the hydrogen sulfide bubbles. Slowly add the solution of 60% hydrochloric acid to the boiling flask. Begin the titration with Mercuric Acetate Titrant until the bright amber color changes to strawberry red. Add enough hydrochloric acid to turn the solution in the boiling flask green, and then let it boil for 15 min. Continue the titration throughout the boiling stage, making sure to rinse the inside of the bubbler with the solution in the beaker by turning off the nitrogen flow until the solution rises to the top of the vertical tube. Rinse the tube a second time (the solution usually returns to amber during the first rinse). Continue the titration and record the volume of titrant used to the nearest 0.01 mL. Calculation The concentration of sulfur in the sample, in mg/kg, is calculated by the following formula: (VS – VB) × K/W, in which VS is the volume, in mL, of titrant to the endpoint for the sample; VB is the volume, in mL, of titrant to the endpoint for the blank (usually about 0.10 mL); K is a constant determined from the calibration of the Sulfur Standard (expressed as µg sulfur per mL titrant); and W is the weight, in g, of the sample. The Sulfur Standards are analyzed, in duplicate, to determine the constant, K, and are calculated by the following formula: K = W × C/(VS – VB), in which W is the weight, in g, of the Sulfur Standard; C is the concentration, in mg/kg, of the Sulfur Standard; VS is the volume, in mL, of titrant for the Sulfur Standard; and VB is the volume, in mL, of titrant for the Titration Reagent Blank. Unsaponifiable Matter Proceed as directed under Unsaponifiable Matter, Appendix VII. Water Proceed as directed under Water Determination using the Karl Fischer Titrimetric Method, Appendix IIB. However, in place of 35 to 40 mL of methanol, use 50 mL of a 1:1 chloroform:methanol mixture to dissolve the sample. Packaging and Storage
Store in well-closed containers.
10 / Carmine / Monographs
FCC IV, Supplement 3
Revision: Description and Assay test corrected.
Carmine Carminic Acid CH2OH OH
H
OH H HO H HO
OH
O
CH3
ima in the range 520–550 nm, when determined in a 1-cm cell with a suitable spectrophotometer against a water blank, and the absorbance at 520 nm is not less than 0.30. Assay Not less than 42.0%1 of carminic acid (C22H20O13), calculated on the dried basis. Arsenic (as As) Not more than 1 mg/kg. Ash Not more than 12.0%. Lead Not more than 10 mg/kg. Loss on Drying Not more than 20.0%. Microbial Limits: Salmonella Negative in 25 g.
COOH
TESTS HO OH
O
OH
C22H20O13
Formula wt 492.39
INS: 120
CAS: [1390-65-4]
DESCRIPTION Carmine is the aluminum or the calcium–aluminum lake, on an aluminum hydroxide substrate, of the coloring principles obtained by an aqueous extraction of cochineal. Cochineal consists of the dried female insects Dactylopius coccus costa (Coccus cacti L.), enclosing young larvae; the coloring principles derived therefrom consist chiefly of carminic acid (C22H20O13). Carminic acid crystallizes from water as bright red crystals that darken at 130° and decompose at 250°; it is freely soluble in water, in alcohol, in ether, in concentrated sulfuric acid, and in solutions of alkali hydroxides; it is insoluble in petroleum ether and in chloroform; its aqueous solutions at pH 4.8 are red-orange to yellow, and at 6.2 are dark red to violet. Carmine occurs as bright red, friable pieces or as a dark red powder. It is soluble in alkali solutions, slightly soluble in hot water, and practically insoluble in cold water and in dilute acids. Before use in food, Carmine must have been pasteurized or otherwise treated to destroy all viable Salmonella microorganisms. According to the pertinent U.S. color additive regulation (21 CFR 73.100), “pasteurization or such other treatment is deemed to permit the adding of safe and suitable substances (other than chemical preservatives) that are essential to the method of pasteurization or other treatment used.” Note: The specifications and tests in this monograph refer to Carmine without any added substances for pasteurization or any other such treatment. Functional Use in Foods
Color.
Assay Accurately weigh about 0.100 g of Carmine (~ 52% carminic acid content), dissolve in 30 mL of 2 N hydrochloric acid, and heat to a boil for 30 s. After cooling, dilute to a volume of 1 L. Determine the absorbance of this solution in a 1-cm cell at the wavelength of maximum absorbance at about 494 nm, with a suitable spectrophotometer, using a 1:3 dilution of 2 N hydrochloric acid as the blank. To obtain accurate results, the absorbance must be in the range of 0.650 to 0.750. Adjust the starting weight as necessary to achieve this absorbance. Calculate the percentage of carminic acid in the sample of Carmine taken by the formula 100 × A/13.9 W, in which A is the absorbance of the sample solution and W is the weight, in g, of the sample taken. Note: If a black or brown precipitate forms, filter the solution. Arsenic, Appendix IIIB Transfer 3.0 g of the sample into a 500mL Kjeldahl flask equipped with a steam trap, add 5 g of ferrous sulfate and 75 mL of hydrochloric acid, and mix. Connect the flask with the steam trap and with a condenser, the delivery tube of which consists of a large-size straight adapter and extends to slightly above the bottom of a 500-mL Erlenmeyer flask containing 100 mL of water. Begin heating the Kjeldahl flask and collect about 40 mL of distillate in the Erlenmeyer flask. Pour the distillate mixture into a 600-mL beaker, add 20 mL of bromine water, and heat on a hot plate until the volume is reduced to about 2 mL. Transfer the residual liquid into a 125-mL arsine generator flask (see Appendix IIIB, Figure 11) with the aid of 35 mL of water, and continue as directed in the Procedure under Arsenic Test, Appendix IIIB, beginning with “Add 20 mL of dilute sulfuric acid (1:5). . . .” Ash Transfer about 1 g of the sample into a tared, previously ignited and cooled porcelain crucible, and ignite with a Meker burner (red-hot) to constant weight.
REQUIREMENTS Identification Mix 333 mg of Carmine with 44 mL of water, 0.15 mL of sodium hydroxide solution (1:10), and 0.2 mL of ammonium hydroxide, warm to dissolve, and dilute to volume with water in a 500-mL volumetric flask. Pipet 10.0 mL of this solution into a 250-mL volumetric flask, dilute to volume with water, and mix. The resulting solution exhibits absorption max-
1The 42.0% minimum content of carminic acid specified herein does not indicate that the FCC-grade product is of any lower quality than that described in the second supplement to FCC II (page 18), which specified 50.0%. Rather, the revised Assay procedure used for this edition gives a more accurate indication of the true carminic acid content.
FCC IV, Supplement 3
Monographs / Cellulose Gum / 11
Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Loss on Drying, Appendix IIC Dry a 1-g sample at 135° for 3 h. Microbial Limits: Salmonella Proceed as directed in chapter 5 of the FDA Bacteriological Analytical Manual, Eighth Edition, 1998. Packaging and Storage cool, dry place.
Store in well-closed containers in a
Revision: Specifications for Degree of Substitution and Sodium modified; Heavy Metals (as Pb) specification and determination deleted.
Cellulose Gum Sodium Carboxymethylcellulose; CMC; Modified Cellulose
O
H
OR
OR H
H
H
H
O CH2OR
n
in which R = H or CH2COONa
INS: 466
CAS: [9004-32-4]
DESCRIPTION It occurs as a white- to cream-colored powder or as granules. The powder is hygroscopic. A 1:100 aqueous suspension has a pH between 6.5 and 8.5. It is readily dispersed in water to form viscous, colloidal solutions. It is insoluble in most solvents. Functional Use in Foods
Thickener; stabilizer.
REQUIREMENTS Identification While stirring, add about 1 g of powdered sample to 50 mL of warm water to produce a uniform dispersion. Continue stirring until a colloidal solution is produced, and then cool to room temperature. Use this solution for tests A and B. A. Add 10 mL of cupric sulfate TS to about 10 mL of the sample solution. A fluffy, bluish white precipitate is formed. B. The sample solution gives a positive test for Sodium, Appendix IIIA. Assay Not less than 99.5% and not more than 100.5% of Cellulose Gum, calculated on the dried basis. Degree of Substitution Not less than 0.2 and not more than 1.50 carboxymethyl groups (—CH2COOH) per anhydroglucose unit after drying. Lead Not more than 3 mg/kg. Loss on Drying Not more than 10.0%.
Sodium Not more than 12.4% after drying. Viscosity of a 2%, Weight in Weight, Solution Not less than 25 mPa·s (equivalent to 25 centipoises). TESTS Assay Calculate the percentage of Cellulose Gum by subtracting from 100 the percentages of Sodium Chloride and Sodium Glycolate determined as follows: Sodium Chloride Accurately weigh about 5 g of the sample, transfer into a 250-mL beaker, add 50 mL of water and 5 mL of 30% hydrogen peroxide, and heat on a steam bath for 20 min, stirring occasionally to ensure complete dissolution. Cool, and using silver and mercurous sulfate–potassium sulfate electrodes and stirring constantly, add 100 mL of water and 10 mL of nitric acid, and titrate with 0.05 N silver nitrate to a potentiometric endpoint. Calculate the percentage of sodium chloride in the sample by the formula 584.4 × V × N/(100 – b) × W, in which V and N represent the volume, in mL, and the normality, respectively, of the silver nitrate; b is the percentage of Loss on Drying, determined separately; W is the weight, in g, of the sample; and 584.4 is an equivalence factor for sodium chloride. Sodium Glycolate Transfer about 500 mg, accurately weighed, of the sample into a 100-mL beaker, moisten thoroughly with 5 mL of glacial acetic acid, followed by 5 mL of water, and stir with a glass rod until solution is complete (usually about 15 min). Slowly add 50 mL of acetone, with stirring, then add 1 g of sodium chloride, and stir for several min to ensure complete precipitation of the Cellulose Gum. Filter through a soft, opentextured paper, previously wetted with a small amount of acetone, and collect the filtrate in a 100-mL volumetric flask. Use an additional 30 mL of acetone to facilitate transfer of the solids and to wash the filter cake, then dilute to volume with acetone, and mix. Prepare a series of standard solutions as follows: Transfer 100 mg of glycolic acid, previously dried in a desiccator at room temperature overnight and accurately weighed, into a 100-mL volumetric flask, dissolve in and dilute to volume with water, and mix. Use this solution within 30 days. Transfer 1.0 mL, 2.0 mL, 3.0 mL, and 4.0 mL of the solution into separate 100-mL volumetric flasks, add sufficient water to each flask to make 5 mL, then add 5 mL of glacial acetic acid, and dilute to volume with acetone. Transfer 2.0 mL of the sample solution and 2.0 mL of each standard solution into separate 25-mL volumetric flasks, and prepare a blank flask containing 2.0 mL of a solution of 5% each of glacial acetic acid and water in acetone. Place the uncovered flasks in a boiling water bath for exactly 20 min to remove the acetone, remove from the bath, and cool. Add to each flask 5.0 mL of 2,7-dihydroxynaphthalene TS, mix thoroughly, add an additional 15 mL, and again mix thoroughly. Cover the mouth of each flask with a small piece of aluminum foil. Place the flasks upright in a boiling water bath for 20 min, then remove from the bath, cool, dilute to volume with sulfuric acid, and mix. Using a suitable spectrophotometer, determine the absorbance of each solution at 540 nm against the blank, and prepare
12 / Citric Acid / Monographs
a standard curve using the absorbance values obtained from the standard solutions. From the standard curve and the absorbance of the sample, determine the weight (w), in mg, of glycolic acid in the sample, and calculate the percentage of sodium glycolate in the sample by the formula 12.9 × w/(100 – b) × W, in which 12.9 is a factor converting glycolic acid to sodium glycolate; b is the percentage of Loss on Drying, determined separately; and W is the weight, in g, of the sample. Degree of Substitution Weigh accurately about 200 mg of the sample, previously dried at 105° to constant weight, and transfer it into a 250-mL glass-stoppered Erlenmeyer flask. Add 75 mL of glacial acetic acid, connect the flask with a water-cooled condenser, and reflux gently on a hot plate for 2 h. Cool, transfer the solution to a 250-mL beaker with the aid of 50 mL of glacial acetic acid, and titrate with 0.1 N perchloric acid in dioxane while stirring with a magnetic stirrer. Determine the endpoint potentiometrically with a pH meter equipped with a standard glass electrode as well as an unsealed calomel electrode that has been modified as follows: Discard the aqueous potassium chloride solution contained in the electrode, rinse with water, and fill with the supernatant liquid obtained by shaking thoroughly 2 g each of potassium chloride and silver chloride (or silver oxide) with 100 mL of methanol, then add a few crystals of potassium chloride and silver chloride (or silver oxide) to the electrode. Record the mL of 0.1 N perchloric acid versus mV (0- to 700-mV range), and continue the titration to a few mL beyond the endpoint. Plot the titration curve, and read the volume (A), in mL, of 0.1 N perchloric acid at the inflection point. Calculate the degree of substitution by the formula (16.2 A/G)/[1.0 – (8.0 A/G)],
FCC IV, Supplement 3
Revision: Description revised; Heavy Metals (as Pb) and Ultraviolet Absorbance specifications and determinations deleted; Tridodecylamine specification revised; Readily Carbonizable Substances test replaced; Residue on Ignition test reworded.
Citric Acid HO
O
O
OH O
HO
C6H8O7 C6H8O7.H2O INS: 330
OH
Formula wt, anhydrous 192.13 Formula wt, monohydrate 210.14 CAS: anhydrous [77-92-9] CAS: monohydrate [5949-29-1]
DESCRIPTION Citric Acid is anhydrous or contains one molecule of water of hydration. It occurs as colorless, translucent crystals or as a white, granular to fine crystalline powder. The hydrous form is efflorescent in dry air. One g is soluble in about 0.5 mL of water, in about 2 mL of alcohol, and in about 30 mL of ether. Functional Use in Foods Sequestrant; dispersing agent; acidifier; flavoring agent. REQUIREMENTS
in which G is the weight, in mg, of the sample taken; 16.2 is onetenth of the molecular weight of one anhydroglucose unit; and 8.0 is one-tenth of the molecular weight of one sodium carboxymethyl group. Lead A Sample Solution prepared from a 2-g sample as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 6 µg of lead ion (Pb) in the control. Loss on Drying, Appendix IIC Dry to constant weight at 105°. Sodium From the weight of the sample and the number of mL of 0.1 N perchloric acid consumed in the determination of Degree of Substitution, calculate the percentage of sodium. Each mL of 0.1 N perchloric acid is equivalent to 2.299 mg of sodium. Viscosity of a 2%, Weight in Weight, Solution Determine as directed under Viscosity of Cellulose Gum, Appendix IIB.
Labeling Indicate whether it is anhydrous or hydrous. Identification A 1:10 solution gives positive tests for Citrate, Appendix IIIA. Assay Not less than 99.5% and not more than 100.5% of C6H8O7, calculated on the anhydrous basis. Lead Not more than 0.5 mg/kg. Oxalate Passes test. Readily Carbonizable Substances Passes test. Residue on Ignition Not more than 0.05%. Tridodecylamine (in solvent-extracted Citric Acid only) Not more than 0.1 mg/kg. Water Anhydrous form: not more than 0.5%; monohydrate form: not more than 8.8%.
Packaging and Storage
TESTS
Store in well-closed containers.
Assay Dissolve about 3 g, accurately weighed, in 40 mL of water, add phenolphthalein TS, and titrate with 1 N sodium hydroxide. Each mL of 1 N sodium hydroxide is equivalent to 64.04 mg of C6H8O7. Lead Determine as directed under the Atomic Absorption Spectrophotometric Graphite Furnace Method, Method I, in the Lead Limit Test, Appendix IIIB. Oxalate Neutralize 10 mL of a 1:10 solution with 6 N ammonium hydroxide, add 5 drops of 2.7 N hydrochloric acid, cool, and add 2 mL of calcium chloride TS. No turbidity is produced.
FCC IV, Supplement 3
Readily Carbonizable Substances Transfer 1.00 ± 0.01 g of finely powdered Citric Acid to a 150-mm × 18-mm (od) tube previously rinsed with 10 mL of 98% sulfuric acid at 90° or used exclusively for this test. Add 10 ± 0.1 mL of 98% sulfuric acid, carefully agitate the tube until solution is complete, and immerse the tube in a water bath at 90° ± 1° for 1 h. Occasionally remove the tube from the water bath and carefully agitate it to ensure that the Citric Acid is dissolved and gaseous decomposition products are allowed to escape to the atmosphere. Cool the tube to ambient temperature, carefully shake the tube to ensure that all gases are removed, and using an adequate spectrophotometer, measure the absorbance and transmission of the solution at 470 nm in a 1-cm cell. The absorbance does not exceed 0.52, and the transmission is equal to or exceeds 30%. Residue on Ignition Determine as directed under Residue on Ignition, Appendix IIC, igniting a 4-g sample. Tridodecylamine (in solvent-extracted Citric Acid only) Buffered Indicator Solution Prepare a mixture consisting of 700 mL of 0.1 M Citric Acid (anhydrous, reagent grade), 200 mL of 0.2 M disodium phosphate, and 50 mL each of 0.2% bromophenol blue and of 0.2% bromocresol green in spectrograde methanol. No-Indicator Buffer Solution Prepare a mixture consisting of 700 mL of 0.1 M Citric Acid (anhydrous, reagent grade), 200 mL of 0.2 M disodium phosphate, and 100 mL of spectrograde methanol. Amine Stock Solution Transfer between 40 and 45 mg of tridodecyl(trilauryl)amine, accurately weighed, into a 500-mL volumetric flask, dilute to volume with isopropyl alcohol, and mix. Discard after 3 weeks. Standard Amine Solution Using a graduated 5-mL pipet, transfer into a 100-mL volumetric flask an amount of Amine Stock Solution equivalent to 400 µg of tridodecylamine, dilute to volume with isopropyl alcohol, and mix. Prepare this solution fresh on the day of use. Procedure Dissolve 160 g of anhydrous reagent-grade Citric Acid (not the sample to be tested) in 320 mL of water, and divide the solution equally between two 250-mL separators, S1 and S2. Add 5 mL of No-Indicator Buffer Solution to S1. Add 2.0 mL of Standard Amine Solution and 5 mL of Buffered Indicator Solution to S2. To prepare solutions of the sample being tested, dissolve 160 g of anhydrous Citric Acid sample in 320 mL of water (or 174 g of Citric Acid monohydrate sample in 306 mL of water). Divide the test solution equally between two 250-mL separators, S3 and S4. Add 5 mL of No-Indicator Buffer Solution to S3, and 5 mL of Buffered Indicator Solution to S4. Add 20 mL of a 1 to 1 mixture (v/v) prepared from spectrograde chloroform and n-heptane to each of the four separators, shake for 15 min on a mechanical shaker, and allow the phases to separate for 45 min. Drain all except the last few drops of the lower (aqueous) phases, and discard. Hand-shake the organic phases with 25 mL each of 0.05 N sulfuric acid for 30 s, and allow the phases to separate for 30 min. Drain all except the last few drops of the lower (organic) phases through dry Whatman No. 40 (or equivalent) paper, and collect the aqueous filtrates in separate small glass-stoppered containers.
Monographs / Cocoa Butter Substitute / 13
Determine the absorbance of each solution in a 5-cm cell at 400 nm, with a suitable spectrophotometer standardized prior to analysis, against chloroform:heptane (1:1 v/v). The net absorbance of the sample (S4 – S3) is not greater than that of the standard (S2 – S1). Water Determine as directed under the Karl Fischer Titrimetric Method, Appendix IIB. Packaging and Storage
Store in tightly closed containers.
Revision: Description corrected, Heavy Metals (as Pb) specification and determination deleted.
Cocoa Butter Substitute
DESCRIPTION Cocoa Butter Substitute occurs as a white, waxy solid that is predominantly a mixture of triglycerides derived primarily from palm, safflower, sunflower, or coconut oils. The resulting products may be used directly or with cocoa butter in all proportions for the preparation of coatings. In contrast to many edible oils and hard butters, Cocoa Butter Substitute has an abrupt melting range, changing from a rather firm, plastic solid below 32° to a liquid at about 33.8° to 35.5°. Functional Use in Foods turizer.
Coating agent; formulation aid; tex-
REQUIREMENTS Identification Cocoa Butter Substitute exhibits the following typical composition profile of fatty acids as determined under Fatty Acid Composition, Appendix VII: Fatty Acid:
≤12
12:0
14:0
16:0
Weight % (Range): 0.0
0.0
0.0
21–24 0.0
Fatty Acid:
18:1
18:2
≥20
18:0
Weight % (Range): 40–44 31–35 0.5–1.5 0.3–0.7 Color (AOCS-Wesson) Not more than 2.5 red. Free Fatty Acids (as oleic acid) Not more than 1.0%. Glycerides Not less than 98.0% of total. Monoglycerides Not more than 1.0%. Diglycerides Not more than 7.0%. Triglycerides Not less than 90.0%. Hexane Not more than 5 mg/kg. Iodine Value Between 30 and 33. Lead Not more than 0.1 mg/kg. Peroxide Value Not more than 10 meq/kg. Residual Catalyst (as F) Not more than 0.5 mg/kg. Unsaponifiable Matter Not more than 1.0%. Water Not more than 0.1%.
16:1
14 / Cocoa Butter Substitute / Monographs
TESTS
FCC IV, Supplement 3
TG = T + D + M,
temperature at 110°, maintain the detectors at 200°, and hold the column oven initially at 70° for 2 min followed by a linear temperature gradient at 5°/min for 22 min at a temperature between 70° and 180° and a final hold at 180° for 10 min or until the column is clean. Standard Curve Chromatograph aliquots of each Standard Preparation as directed under Procedure. Measure the peak areas for each Standard Preparation. Plot a standard curve using the concentration, in mg/kg, of each Standard Preparation versus its corresponding peak area, and draw the best straight line. Procedure Insert the Assay Preparation into the inlet liner of the gas chromatograph, immediately sealing the base of the inlet and the lower lip of the glass tubing with a silicone O-ring (Applied Science Laboratories, Inc., or equivalent) previously heated at 200° for 2 h to remove volatile impurities. Immediately close the inlet liner with the septum and septum liner. Allow the carrier gas to flow through the Assay Preparation, chromatograph as directed under Chromatographic System, and record the chromatograms. Using the peak area of hexane eluting from the Assay Preparation at the same time as the Standard Preparation, read directly from the Standard Curve the concentration, C, of hexane, in mg/kg, of the Assay Preparation. Calculate the quantity, in mg/ kg, of hexane in the sample by the formula
T = WT100/WU,
25C/W,
D = (WD100/WU) – F,
in which W is the weight, in mg, of the sample introduced into the gas chromatograph. Iodine Value Determine as directed under Iodine Value, Appendix VII. Lead Determine as directed for Method II in the Atomic Absorption Spectrophotometric Graphite Furnace Method under the Lead Limit Test, Appendix IIIB, using a 5-g sample. Peroxide Value Determine as directed in Method II under Peroxide Value, Appendix VII; however, after adding the saturated solution of potassium iodide, mix for 1 min, add 200 mL of water, and titrate with 0.05 N sodium thiosulfate, adding starch TS as the endpoint is approached, and continue the titration until the blue starch color has just disappeared. Perform a blank determination (see General Provisions), and make any necessary correction. Proceed with the calculation shown in the appendix. Residual Catalyst Transfer a 30-g sample, accurately weighed, into a 250-mL distillation flask having a side arm and a trap. Connect the flask with a condenser, and fit it with a thermometer and a capillary tube. Both of these should reach nearly to the bottom of the flask so that they extend into the liquid during the distillation. Add 0.2 g of silver sulfate, three boiling beads, and 25 mL of 1:1 aqueous dilution of sulfuric acid to the flask. Connect a dropping funnel or a steam generator to the capillary tube. Distill until the temperature reaches 135°. Then, through the capillary, add water from the funnel, or introduce steam, as necessary, to maintain the temperature as close to 135° as possible until 250 mL of distillate has been collected in a beaker. Cool the distillate. Add 3 mL of 30% hydrogen peroxide to remove any sulfites, let stand for 5 min, and evaporate the distillate in a dish containing 15 mL of saturated calcium hydroxide suspension. Ash the residue at 600° for 4 h. Using the ashed residue as the sample, proceed as directed in Method I under Fluoride Limit Test, Appendix IIIB, beginning with “. . . and 30 mL of water in a 125-mL distillation flask having a side arm and trap.” The total volume of sodium
Color (AOCS-Wesson) Determine as directed under Color (AOCS-Wesson), Appendix VII. Free Fatty Acids (as oleic acid) Using the diglyceride fraction under Glycerides (below), proceed as directed under Free Fatty Acids, Appendix VII, except add 2 mL of phenolphthalein TS, and titrate with the appropriate normality of sodium hydroxide. Use the following equivalence factor (e) in the formula given in the procedure: Free fatty acids as oleic acid, e = 28.2. Glycerides Determine as directed under Total Monoglycerides, Appendix VII, except save all three elution fractions to determine the percentages of Monoglycerides, Diglycerides, and Triglycerides. Note: Use toluene instead of benzene. The diglyceride fraction also contains free fatty acids, the percentage of which is determined under Free Fatty Acids. Calculate the percentage of Glycerides, which is the sum of Monoglycerides, Diglycerides, and Triglycerides, by the following formulas:
M = WM100/WU, in which TG is the percent of total glycerides; T is the percent of triglycerides; D is the percent of diglycerides; M is the percent of monoglycerides; WT is the weight, in g, of triglycerides; WU is the weight, in g, of the sample taken; WD is the weight, in g, of diglycerides; F is the percent of free fatty acids; and WM is the weight, in g, of monoglycerides. Hexane Standard Preparation Using a micropipet, transfer 34 µL of hexane into 45 g of cold-pressed cottonseed oil (that has not been extracted with hexane), and dissolve. As directed under Procedure, analyze aliquots of 0.1, 0.25, 0.5, and 5.0 mg; the aliquots correspond to 2, 5, 10, and 100 mg/kg, respectively, of residual hexane in a 25-mg sample. Assay Preparation Pack the lower half of 8.5-cm × 9.5-mm (od) borosilicate glass tubing (inlet liner) with glass wool that has been heated at 200° for 16 h to expel volatiles. Transfer a 25-mg sample, accurately weighed, into the glass tubing, and cover it with a small plug of treated glass wool. Chromatographic System Use a suitable gas chromatograph that is equipped with independent dual flame-ionization detectors and contains a 0.6-m × 6.35-mm (od) stainless-steel Utube packed with Porapak P or equivalent. Use helium as the carrier gas at a flow rate of 60 mL/min, hydrogen as the fuel gas at a flow rate of 52 mL/min for each flame, and air as the scavenger gas for both flames at a flow rate of 500 mL/min. To ensure that the relative standard deviation does not exceed 2.0%, chromatograph a sufficient number of replicates of each Standard Preparation, and record the areas as directed under Procedure (see Chromatography, Appendix IIA). Insert the Assay Preparation into the chromatograph, and subject it to the following operating conditions: Maintain the inlet
FCC IV, Supplement 3
Monographs / Curdlan / 15
fluoride TS required for the solutions from both Distillate A and Distillate B should not exceed 0.75 mL. Unsaponifiable Matter Determine as directed under Unsaponifiable Matter, Appendix VII. Water Proceed as directed under Water Determination, Appendix IIB. However, in place of 35 to 40 mL of methanol, use 50 mL of a 1:1 chloroform:methanol mixture to dissolve the sample. Packaging and Storage
Lead Not more than 0.5 mg/kg. Loss on Drying Not more than 10%. Microbial Limits Aerobic Plate Count Not more than 1000 CFU per g. E. coli Negative in 1 g. Nitrogen Not more than 0.3%. pH (1% aqueous suspension) Between 6.0 and 7.5. Residue on Ignition Not more than 6%.
Store in well-closed containers. TESTS
This is a new monograph:
Curdlan beta-1,3-glucan CH2OH O OH OH OH
CH2OH O O OH
OH
CH2OH OH O O OH n
OH
(C6H10O5)n CAS [54724-00-4]
DESCRIPTION
Curdlan content (%) = (A/AR) × (0.9 × WR/W) × 100,
Curdlan occurs as a white to nearly white powder. It is a highmolecular-weight polymer of glucose (β-1,3-glucan), produced by pure culture fermentation of a carbohydrate by a nonpathogenic and nontoxigenic strain of Agrobacterium biobar 1 (formerly Alcaligenes faecalis var. myxogenes) or Agrobacterium radiobacter. Curdlan consists of β-(1,3)-linked glucose residues and has the unusual property of forming an elastic gel when its aqueous suspension is heated to a temperature above 54°. It is insoluble in water but soluble in alkaline solutions. Functional Use in Foods lizer; thickener.
Assay Sample Solution Transfer about 100 mg of the sample, accurately weighed, into a 100-mL volumetric flask, and dissolve in about 90 mL of 0.1 N sodium hydroxide. Add 0.1 N sodium hydroxide to volume, and mix well. Transfer 5 mL of the solution into a 100-mL volumetric flask, add water to volume, and mix well. Add 1 mL of a 5:100 solution of reagent-grade phenol and 5 mL of sulfuric acid TS to 1 mL of the solution, shake vigorously, and cool in ice-cold water. Prepare a blank and a Reference Standard Solution in the same manner, using 0.1 mL of water and 100 mg of reagent-grade glucose, respectively. Procedure Determine the absorbance of the Sample Solution and the Reference Standard Solution in 1-cm cells, at 490 nm, with a suitable spectrophotometer, using the blank solution to zero it. Calculation Calculate the content of Curdlan in the sample, in percent, using the following equation:
Firming agent; gelling agent; stabi-
REQUIREMENTS Identification A. Add 5 mL of sulfuric acid TS to 10 mL of a 2% aqueous suspension of the sample, heat in a boiling water bath for 30 min, and cool. Neutralize the mixture with barium carbonate, and centrifuge it at 900 g for 10 min. Add 1 mL of the supernatant to 5 mL of hot alkaline cupric tartrate TS. A copious red precipitate of cuprous oxide is formed. B. Heat a 2% aqueous suspension of the sample in a boiling water bath for 10 min and cool. A firm gel forms. C. Suspend 0.2 g of the sample in 5 mL of water, add 1 mL of 3 N sodium hydroxide, and shake. The sample dissolves. Assay Not less than 80% (calculated as anhydrous glucose). Gel Strength (2% aqueous suspension) Not less than 600 g/ cm2.
in which A is the absorbance of the Sample Solution; AR is the absorbance of the Reference Standard Solution; 0.9 is the molecular weight of anhydrous glucose divided by the molecular weight of glucose; WR is the weight, in mg, of the glucose standard used as reference; and W is the weight, in mg, of the sample. Gel Strength Procedure Place 200 mg of the sample into the tube of a Potter-Elvehjem homogenizer, add 10 mL of water, and homogenize at about 1500 g for 5 min. Transfer the suspension into a 16mm × 150-mm test tube, de-aerate in vacuum for 3 min, and heat in a boiling water bath for 10 min to form a gel. Cool in running water, let stand for 30 min, then remove the gel from the test tube. Cut the gel accurately at distances of 20 mm and 30 mm from the bottom to obtain a section 10 mm long. Determine the gel strength using a Rheo Meter Model CR-200D (Sun Scientific Co., Ltd., Japan; Load cell: 1000 g; set to a measurement mode 4) or an equivalent instrument capable of uniaxial compression and having a load cell sensitivity of 500 to 1000 g. Use a cylindrical stainless steel plunger having a 0.5-cm diameter. Lower the plunger into the gel at 250 mm/min. The resulting force–time curve is recorded and used for gel strength calculation. Calculation Calculate gel strength by the following equation: Gel strength (g force/cm2) = f/0.196 cm2, in which f is the force on the force–time curve that shows a sharp yielding downward trend associated with rupture of the gel, and 0.196 is the area, in cm2, of the plunger.
16 / gamma-Cyclodextrin / Monographs
FCC IV, Supplement 3
Lead Determine as directed for Method II in the Atomic Absorption Spectrophotometric Graphite Furnace Method under the Lead Limit Test, Appendix IIIB. Loss on Drying Determine as directed under Loss on Drying, Appendix IIC, drying in a vacuum for 5 h at 60º. Microbial Limits Aerobic Plate Count Determine as directed in chapter 3 of the FDA Bacteriological Analytical Manual, Eighth Edition, 1998. E. coli Determine as directed in chapter 4 of the FDA Bacteriological Analytical Manual, Eighth Edition, 1998. Nitrogen Determine as directed for Method II under Nitrogen Determination, Appendix IIIC, using a 1-g sample. pH Determine as directed under pH Determination, Appendix IIB, using a 2% aqueous suspension. Residue on Ignition Determine as directed for Method I under Residue on Ignition, Appendix IIC, using a 1-g sample. Packaging and Storage
Store in airtight containers.
This is a new monograph:
Cyclodextrin is freely soluble in water and very slightly soluble in ethanol. Functional Use in Foods lation aid.
Stabilizer; emulsifier; carrier; formu-
REQUIREMENTS Identification The infrared absorption spectrum of the sample exhibits relative maxima (that may vary in intensity) at the same wavelengths (or frequencies) as those shown in the respective spectrum in the section on Infrared Spectra, using the same test conditions as specified therein. Assay Not less than 98.0% as gamma-Cyclodextrin on the anhydrous basis. Iodine Reaction A clear brown solution is formed. Lead Not more than 1 mg/kg. Optical Rotation [α]25° D : Between +174° and +180° in a 1% solution. Reducing Sugars (as glucose) Not more than 0.5%. Residue on Ignition Not more than 0.1%. Volatile Organic Compounds Not more than 20 mg/kg. Water Not more than 11.0%.
gamma-Cyclodextrin
TESTS
γ-Cyclodextrin; gamma-CD; Cyclooctaamylose; Cyclomaltooctaose
Assay Sample Solution Transfer 1.0 g, accurately weighed, into a 100-mL flask, dilute to volume with water, and mix. Chromatographic System Determine as directed under Chromatography, Appendix IIA, but use a liquid chromatograph equipped with a differential refractometer detector, a 7.8-mm id × 30-cm column packed with 25-µm silver bonded to sulfonated divinyl benzene–styrene copolymer (Aminex HPX-42A, Bio-Rad Laboratories, or equivalent). Maintain the column at a constant temperature of 65° ± 10°, and the flow rate at 0.3 to 1.0 mL/min. Use water as the mobile phase. Procedure Inject about 20 µL of the Sample Preparation into the chromatograph, record the chromatogram, and measure the responses for all peaks. Calculation Calculate the content of gamma-Cyclodextrin in the sample by the peak area percentage method using the following formula:
OH OH
O
H O H
O
O
O O
2O
O
O H HOH2C 2C O
O
H
O
OH OH
(C6H10O5)8
OH OH
H
H O H
2C
CH
O
O O H
OH OH
HOH2C
O
O
O
O
2O
H
H
CH2OH
OH OH
H
O CH2OH
OH OH
OC
A = (B/C) × 100,
O
Formula wt 1297 CAS: [17465-86-0]
DESCRIPTION Gamma-Cyclodextrin is a nonreducing cyclic saccharide consisting of eight α-1,4-linked D-glucopyranosyl units manufactured by the action of cyclomaltodextrin glucanotransferase on hydrolyzed starch followed by purification of the gamma-Cyclodextrin. It occurs as a white or almost-white crystalline solid. Gamma-
in which A is the percentage of gamma-Cyclodextrin in the sample, B is the peak area of gamma-Cyclodextrin in the chromatogram, and C is the sum of the areas of all peaks recorded in the chromatogram. Iodine Reaction Place 0.2 g of the sample in a test tube, and add 2 mL of a 0.1 N iodine solution. Heat the mixture in a water bath, and allow to cool at room temperature. Lead Reflux about 5 g of the sample, accurately weighed, with 30 mL of nitric acid for 1 h. Remove the reflux condenser, and attach a condenser to the flask. Continue to heat, and collect the distilled nitric acid. Allow the residue to cool, add 20 mL of water, and allow to cool again. Add 2 mL of orthophosphoric acid, dilute to 100 mL with water, and determine the lead content of the
FCC IV, Supplement 3
in which V1 and N1 are the volume, in mL, and the normality, respectively, of the iodine solution; V2 and N2 are the volume, in mL, and the normality, respectively, of the sodium thiosulfate solution; 2.7 is an empirically determined equivalence factor for D-glucose; and W is the sample weight, in g. Residue on Ignition Proceed as directed under Residue on Ignition (Sulfated Ash), Method I (for Solids), Appendix IIC. Volatile Organic Compounds Dissolve 50 g of the sample in about 700 mL of water in a 1-L round-bottom flask, and add a magnetic stirrer. Attach the flask to the lower part of a Bleidner apparatus (see Figure 1), and connect a 100-mL round-bottom flask containing about 70 mL of hexane and a few boiling stones to the other side of the apparatus. Fill the Bleidner apparatus with equal amounts of water and hexane, and place a reflux condenser on the top. Heat both flasks with heating mantels to boiling. Using the magnetic stirrer, stir the contents of the 1-L flask well. Keep the content of the two flasks boiling for 8 h. After cooling, remove the 100-mL flask, transfer the contents to a 100-mL volumetric flask, and fill that flask to volume with hexane. Analyze the hexane solution as directed under Gas Chromatography, Appendix IIA, with the following conditions: The gas chromatograph is equipped with a flame ionization detector and a 30-m × 0.32-mm (id) column with a stationary phase consisting of 0.25-µm, cross-bonded, 95% dimethyl 5% diphenyl polysiloxane (JBW Scientific DB-5.625, or equivalent). Set the injector to 280°, and hold the temperature at 70° for 4 min, and then increase it to 250° at intervals of 10° per min. Use nitrogen gas as a carrier flowing at 70 mL per min. The detection is FID at 280°. Calculate the area(s) under the peak for each volatile organic compound, and convert it to mg/kg gamma-Cyclodextrin using the response factor 8-cyclohexadecen-1-one. The response factor is determined from a calibration curve using 8-cyclohexadecen-1one concentrations of 0.1 to 6 mg/100 mL hexane. Water Proceed as directed under Water Determination using the Karl Fischer Titrimetric Method, Appendix IIB. Packaging and Storage Store in tight containers in a dry place.
100 mm
20
12
210 mm
60 mm
14
68°
T 29/32 S 4
9 14 95 mm
%R = [(V1N1 – V2N2) × 2.7]/W,
T 29/32 S
50mm
solution as directed under Atomic Absorption Spectrophotometric Graphite Furnace Method, Method I, in Appendix IIIB. Optical Rotation Proceed as directed under Optical (Specific) Rotation, Appendix IIB. Reducing Sugars (as glucose) Transfer about 1 g of the sample, accurately weighed, into a 250-mL Erlenmeyer flask, dissolve in 10 mL of water, and add 25 mL of alkaline cupric citrate TS, and cover the flask with a small beaker. Boil gently for exactly 5 min, and cool rapidly to room temperature. Add 25-mL of 10% acetic acid solution, 10.0 mL of 0.1 N iodine, 10 mL of dilute hydrochloric acid TS, and 3 mL of starch TS, and titrate with 0.1 N sodium thiosulfate to the disappearance of the blue color. Calculate the content of reducing substances (as D-glucose) (R) by the equation
Monographs / Enzyme Preparations / 17
180
FIGURE 1 Bleidner Apparatus.
Revision: Classifications and reactions added for ␣Acetolactatedecarboxylase; Aminopeptidase, Leucine; and Lysozyme; Heavy Metals (as Pb) specification and determination deleted from Additional Requirements.
Enzyme Preparations
DESCRIPTION Enzyme Preparations used in food processing are derived from animal, plant, or microbial sources (see CLASSIFICATION, below). They may consist of whole cells, parts of cells, or cell-free extracts of the source used, and they may contain one active component or, more commonly, a mixture of several, as well as food-grade diluents, preservatives, antioxidants, and other substances consistent with good manufacturing practice. The individual preparations usually are named according to the substance to which they are applied, such as Protease or
18 / Enzyme Preparations / Monographs
Amylase. Traditional names such as Malt, Pepsin, and Rennet also are used, however. The color of the preparations—which may be liquid, semiliquid, or dry—may vary from virtually colorless to dark brown. The active components consist of the biologically active proteins, which are sometimes conjugated with metals, carbohydrates, and/ or lipids. Known molecular weights of the active components range from approximately 12,000 to several hundred thousand. The activity of enzyme preparations is measured according to the reaction catalyzed by individual enzymes (see below) and is usually expressed in activity units per unit weight of the preparation. In commercial practice (but not for Food Chemicals Codex purposes), the activity of the product is sometimes also given as the quantity of the preparation to be added to a given quantity of food to achieve the desired effect. Additional information relating to the nomenclature and the sources from which the active components are derived is provided in the General Tests section under Enzyme Assays, Appendix V. Functional Use in Foods below).
Enzyme (see discussion under CLAS-
SIFICATION,
FCC IV, Supplement 3
Phospholipase A2 Obtained from porcine pancreatic tissue. Produced as a white to tan powder or pale- to dark-yellow liquid. Major active principle: phospholipase A2. Typical application: hydrolysis of lecithins. Rennet, Bovine Aqueous extracts made from the fourth stomach of bovine animals. Clear, amber to dark-brown liquid or white to tan powder. Major active principle: protease (pepsin). Typical application: manufacture of cheese. Similar preparations can be made from the fourth stomach of sheep or goats. Rennet, Calf Aqueous extracts made from the fourth stomach of calves. Clear, amber to dark-brown liquid or white to tan powder. Major active principle: protease (chymosin). Typical application: manufacture of cheese. Similar preparations can be made from the fourth stomach of lambs or kids. Trypsin Obtained from purified extracts of porcine or bovine pancreas. White to tan, amorphous powders soluble in water but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: trypsin. Typical applications: baking; tenderizing of meat; production of protein hydrolysates. Plant-Derived Preparations
CLASSIFICATION Animal-Derived Preparations Catalase (bovine liver) Partially purified liquid or powdered extracts from bovine liver. Major active principle: catalase. Typical application: manufacture of certain cheeses. Chymotrypsin Obtained from purified extracts of bovine or porcine pancreatic tissue. White to tan, amorphous powders soluble in water but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: chymotrypsin. Typical application: hydrolysis of protein. Lipase, Animal Obtained from two primary sources: (1) edible forestomach tissue of calves, kids, or lambs, and (2) animal pancreatic tissue. Produced as purified edible tissue preparations or as aqueous extracts. Dispersible in water; insoluble in alcohol. Major active principle: lipase. Typical applications: manufacture of cheese; modification of lipids. Lysozyme Obtained from extracts of purified chicken egg whites. Generally prepared and used in the hydrochloride form as a white, odorless powder. Major active principle: lysozyme. Typical application: antimicrobial in food processing. Pancreatin Obtained from porcine or bovine (ox) pancreatic tissue. White to tan, water-soluble powder. Major active principles: (1) α-amylase, (2) protease, and (3) lipase. Typical applications: preparation of precooked cereals, infant foods, protein hydrolysates. Pepsin Obtained from the glandular layer of hog stomach. White to light-tan, water-soluble powder; amber paste; or clear amber to brown aqueous liquids. Major active principle: pepsin. Typical applications: preparation of fish meal and other protein hydrolysates; clotting of milk in manufacture of cheese (in combination with rennet).
Amylase Obtained from extraction of ungerminated barley. Clear, amber to dark-brown liquid or white to tan powder. Major active principle: β-amylase. Typical applications: production of alcoholic beverages and sugar syrups. Bromelain The purified proteolytic substance derived from the pineapples Ananas comosus and Ananas bracteatus L. White to light-tan, amorphous powder. Soluble in water (the solution is usually colorless to light yellow and somewhat opalescent) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: bromelain. Typical applications: chillproofing of beer; tenderizing of meat; preparation of precooked cereals; production of protein hydrolysates; baking. Ficin The purified proteolytic substance derived from the latex of Ficus sp., which include a variety of tropical fig trees. White to off-white powders completely soluble in water. (Liquid fig latex concentrates are light brown to dark brown.) Major active principle: ficin. Typical applications: chillproofing of beer; tenderizing of meat; conditioner of dough in baking. Malt The product of the controlled germination of barley. Clear, amber to dark-brown liquid preparations or white to tan powder. Major active principles: (1) α-amylase and (2) β-amylase. Typical applications: baking; manufacture of alcoholic beverages; manufacture of syrups. Papain The purified proteolytic substance derived from the fruit of the papaya Carica papaya L. (Fam. Caricaceae). Produced as a white to light-tan, amorphous powder or a liquid. Soluble in water (the solution is usually colorless or light yellow and somewhat opalescent) but practically insoluble in alcohol, in chloroform, and in ether. Major active principles: (1) papain and (2) chymopapain. Typical applications: chillproofing of beer; tenderizing of meat; preparation of precooked cereals; production of protein hydrolysates.
FCC IV, Supplement 3
Microbially Derived Preparations
Monographs / Enzyme Preparations / 19
␣-Acetolactatedecarboxylase (Bacillus subtilis containing a Bacillus brevis gene) Produced as a brown liquid by controlled fermentation using the modified Bacillus subtilis. Soluble in water (the solution is usually a light yellow to brown). Major active principle: decarboxylase. Typical application: preparation of beer.
Carbohydrase (Bacillus subtilis containing a Bacillus megaterium α-amylase gene) Produced as an off-white to brown, amorphous powder or liquid by controlled fermentation using the modified Bacillus subtilis. Soluble in water (the solution is usually light yellow to dark brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: αamylase. Typical applications: preparation of starch syrups, alcohol, beer, and dextrose.
Aminopeptidase, Leucine (Aspergillus niger var., Aspergillus oryzae var., and other microbial species) Produced as a light-tan to brown powder or as a brown liquid by controlled fermentation using Aspergillus niger var., Aspergillus oryzae var., or other microbial species. The powder is soluble in water (the solution is usually light yellow to brown). Major active principles: (1) aminopeptidase, (2) protease, and (3) carboxypeptidase activities in varying amounts. Typical applications: preparation of protein hydrolysates, development of flavors in processed foods.
Carbohydrase (Bacillus subtilis containing a Bacillus stearothermophilus α-amylase gene) Produced as an off-white to brown, amorphous powder or a liquid by controlled fermentation using the modified Bacillus subtilis. Soluble in water (the solution is usually light yellow to dark brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: maltogenic amylase. Typical applications: preparation of starch syrups, dextrose, alcohol, beer, and baked goods.
Carbohydrase (Aspergillus niger var., including Aspergillus aculeatus) Produced as an off-white to tan powder or a tan to dark-brown liquid by controlled fermentation using Aspergillus niger var. (including Aspergillus aculeatus). Soluble in water (the solution is usually light yellow to dark brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principles: (1) α-amylase, (2) pectinase (a mixture of enzymes, including pectin depolymerase, pectin methyl esterase, pectin lyase, and pectate lyase), (3) cellulase, (4) glucoamylase (amyloglucosidase), (5) amylo-1,6-glucosidase, (6) hemicellulase (a mixture of enzymes, including poly(galacturonate) hydrolase, arabinosidase, mannosidase, mannanase, and xylanase), (7) lactase, (8) β-glucanase, (9) β-D-glucosidase, (10) pentosanase, and (11) α-galactosidase. Typical applications: preparation of starch syrups and dextrose, alcohol, beer, ale, fruit juices, chocolate syrups, bakery products, liquid coffee, wine, dairy products, cereals, and spice and flavor extracts. Carbohydrase (Aspergillus oryzae var.) Produced as an offwhite to tan, amorphous powder or a liquid by controlled fermentation using Aspergillus oryzae var. Soluble in water (the solution is usually light yellow to dark brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principles: (1) α-amylase, (2) glucoamylase (amyloglucosidase), and (3) lactase. Typical applications: preparation of starch syrups, alcohol, beer, ale, bakery products, and dairy products. Carbohydrase (Bacillus acidopullulyticus) Produced as an offwhite to brown, amorphous powder or a liquid by controlled fermentation using Bacillus acidopullulyticus. Soluble in water (the solution is usually light yellow to dark brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: pullulanase. Typical applications: hydrolysis of amylopectins and other branched polysaccharides. Carbohydrase (Bacillus stearothermophilus) Produced as an off-white to tan powder or a light-yellow to dark-brown liquid by controlled fermentation using Bacillus stearothermophilus. Soluble in water but practically insoluble in alcohol, in ether, and in chloroform. Major active principle: α-amylase. Typical applications: preparation of starch syrups, alcohol, beer, dextrose, and bakery products.
Carbohydrase (Candida pseudotropicalis) Produced as an offwhite to tan, amorphous powder or a liquid by controlled fermentation using Candida pseudotropicalis. Soluble in water (the solution is usually light yellow to dark brown) but insoluble in alcohol, in chloroform, and in ether. Major active principle: lactase. Typical applications: manufacture of candy and ice cream; modification of dairy products. Carbohydrase (Kluyveromyces marxianus var. lactis) Produced as an off-white to tan, amorphous powder or a liquid by controlled fermentation using Kluyveromyces marxianus var. lactis. Soluble in water (the solution is usually light yellow to dark brown) but insoluble in alcohol, in chloroform, and in ether. Major active principle: lactase. Typical applications: manufacture of candy and ice cream; modification of dairy products. Carbohydrase (Mortierella vinaceae var. raffinoseutilizer) Produced as an off-white to tan powder or as pellets by controlled fermentation using Mortierella vinaceae var. raffinoseutilizer. Soluble in water (pellets may be insoluble in water) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: α-galactosidase. Typical application: production of sugar from sugar beets. Carbohydrase (Rhizopus niveus) Produced as an off-white to brown, amorphous powder or a liquid by controlled fermentation using Rhizopus niveus. Soluble in water (the solution is usually light yellow to dark brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principles: (1) α-amylase and (2) glucoamylase. Typical application: hydrolysis of starch. Carbohydrase (Rhizopus oryzae var.) Produced as a powder or a liquid by controlled fermentation using Rhizopus oryzae var. Soluble in water but practically insoluble in alcohol, in chloroform, and in ether. Major active principles: (1) α-amylase, (2) pectinase, and (3) glucoamylase (amyloglucosidase). Typical applications: preparation of starch syrups and fruit juices, vegetable purees, and juices; manufacture of cheese. Carbohydrase (Saccharomyces species) Produced as a white to tan, amorphous powder by controlled fermentation using a number of species of Saccharomyces traditionally used in the manufacture of food. Soluble in water (the solution is usually light
20 / Enzyme Preparations / Monographs
yellow) but practically insoluble in alcohol, in chloroform, and in ether. Major active principles: (1) invertase and (2) lactase. Typical applications: manufacture of candy and ice cream; modifications of dairy products. Carbohydrase (Trichoderma longibrachiatum var.; formerly reesei) Produced as an off-white to tan, amorphous powder or a liquid by controlled fermentation using Trichoderma longibrachiatum var. Soluble in water (the solution is usually tan to brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principles: (1) cellulase (2) β-glucanase, (3) β-Dglucosidase, (4) hemicellulase, and (5) pentosanase. Typical applications: preparation of fruit juices, wine, vegetable oils, beer, and baked goods. Carbohydrase and Protease, Mixed (Bacillus licheniformis var.) Produced as an off-white to brown, amorphous powder or a liquid by controlled fermentation using Bacillus licheniformis var. Soluble in water (the solution is usually light yellow to dark brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principles: (1) α-amylase and (2) protease. Typical applications: preparation of starch syrups, alcohol, beer, dextrose, fish meal, and protein hydrolysates. Carbohydrase and Protease, Mixed (Bacillus subtilis var. including Bacillus amyloliquefaciens) Produced as an off-white to tan, amorphous powder or a liquid by controlled fermentation using Bacillus subtilis var. Soluble in water (the solution is usually light yellow to dark brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principles: (1) α-amylase, (2) β-glucanase, (3) protease, and (4) pentosanase. Typical applications: preparation of starch syrups, alcohol, beer, dextrose, bakery products, fish meal; tenderizing of meat; preparation of protein hydrolysates.
FCC IV, Supplement 3
Microbacteruim arborescens, Streptomyces rubiginosus var., or Streptomyces murinus) Produced as an off-white to tan, brown, or pink, amorphous powder, granules, or a liquid by controlled fermentation using any of the above-named organisms. The products may be soluble in water but practically insoluble in alcohol, in chloroform, and in ether, or if immobilized, may be insoluble in water and partially soluble in alcohol, in chloroform, and in ether. Major active principle: glucose (or xylose) isomerase. Typical applications: manufacture of high-fructose corn syrup and other fructose starch syrups. Glucose Oxidase (Aspergillus niger var.) Produced as a yellow to brown solution or as a yellow to tan or off-white powder by controlled fermentation using Aspergillus niger var. Soluble in water (the solution is usually light yellow to brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principles: (1) glucose oxidase and (2) catalase. Typical applications: removal of sugar from liquid eggs; deoxygenation of citrus beverages. Lipase (Aspergillus niger var.) Produced as an off-white to tan, amorphous powder by controlled fermentation using Aspergillus niger var. Soluble in water (the solution is usually light yellow) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: lipase. Typical application: hydrolysis of lipids (e.g., fish oil concentrates and cereal derived lipids). Lipase (Aspergillus oryzae var.) Produced as an off-white to tan, amorphous powder or a liquid by controlled fermentation using Aspergillus oryzae var. Soluble in water (the solution is usually light yellow) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: lipase. Typical applications: hydrolysis of lipids (e.g., fish oil concentrates); manufacture of cheese and cheese flavors.
Catalase (Aspergillus niger var.) Produced as an off-white to tan, amorphous powder or a liquid by controlled fermentation using Aspergillus niger var. Soluble in water (the solution is usually tan to brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: catalase. Typical applications: manufacture of cheese, egg products, and soft drinks.
Lipase (Candida rugosa; formerly Candida cylindracea) Produced as an off-white to tan powder by controlled fermentation using Candida rugosa. Soluble in water but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: lipase. Typical applications: hydrolysis of lipids, manufacture of dairy products and confectionery goods, development of flavor in processed foods.
Catalase (Micrococcus lysodeikticus) Produced by controlled fermentation using Micrococcus lysodeikticus. Soluble in water (the solution is usually light yellow to dark brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: catalase. Typical application: manufacture of cheese, egg products, and soft drinks.
Lipase (Rhizomucor (Mucor) miehei) Produced as an off-white to tan powder or a liquid by controlled fermentation using Rhizomucor miehei. Soluble in water (the solution is usually light yellow to dark brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: lipase. Typical applications: hydrolysis of lipids; manufacture of cheese; removal of haze in fruit juices.
Chymosin (Aspergillus niger var. awamori, Escherichia coli K12, and Kluyveromyces marxianus, each microorganism containing a calf prochymosin gene) Produced as a white to tan, amorphous powder or as a light-yellow to brown liquid by controlled fermentation using the above-named genetically modified microorganisms. The powder is soluble in water but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: chymosin. Typical application: manufacture of cheese; preparation of milk-based desserts. Glucose Isomerase (Actinoplanes missouriensis, Bacillus coagulans, Streptomyces olivaceus, Streptomyces olivochromogenes,
Phytase (Aspergillus niger var.) Produced as an off-white to brown powder or as a tan to dark-brown liquid by controlled fermentation using Aspergillus niger var. Soluble in water but practically insoluble in alcohol, in chloroform, and in ether. Major active principles: (1) 3-phytase and (2) acid phosphatase. Typical applications: soy protein isolate production; phytic acid removal from plant materials. Protease (Aspergillus niger var.) Produced by controlled fermentation using Aspergillus niger var. The purified enzyme occurs as an off-white to tan, amorphous powder. Soluble in water
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Monographs / Enzyme Preparations / 21
(the solution is usually light yellow) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: protease. Typical application: production of protein hydrolysates. Protease (Aspergillus oryzae var.) Produced by controlled fermentation using Aspergillus oryzae var. The purified enzyme occurs as an off-white to tan, amorphous powder. Soluble in water (the solution is usually light yellow) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: protease. Typical applications: chillproofing of beer; production of bakery products; tenderizing of meat; production of protein hydrolysates; development of flavor in processed foods. Rennet, Microbial (nonpathogenic strain of Bacillus cereus) Produced as a white to tan, amorphous powder or a light-yellow to dark-brown liquid by controlled fermentation using Bacillus cereus. Soluble in water but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: protease. Typical application: manufacture of cheese. Rennet, Microbial (Endothia parasitica) Produced as an offwhite to tan, amorphous powder or a liquid by controlled fermentation using nonpathogenic strains of Endothia parasitica. The powder is soluble in water (the solution is usually tan to dark brown) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: protease. Typical application: manufacture of cheese. Rennet, Microbial (Rhizomucor (Mucor) sp.) Produced as a white to tan, amorphous powder by controlled fermentation using Rhizomucor miehei, or pusillus var. Lindt. The powder is soluble in water (the solution is usually light yellow) but practically insoluble in alcohol, in chloroform, and in ether. Major active principle: protease. Typical application: manufacture of cheese. REACTIONS CATALYZED Note: The reactions catalyzed by any given active component are essentially the same, regardless of the source from which that component is derived. ␣-Acetolactatedecarboxylase lactate to acetoin.
Decarboxylation of α-aceto-
Aminopeptidase, Leucine Hydrolysis of N-terminal amino acid, which is preferably leucine, but may be other amino acids, from proteins and oligopeptides, yielding free amino acids and oligopeptides of lower molecular weight.
Cellulase Hydrolysis of β-1,4-glucan bonds in such polysaccharides as cellulose, yielding β-dextrins. Chymosin (calf and fermentation derived) bond in kappa-casein.
Cleaves a single
Ficin Hydrolysis of polypeptides, amides, and esters (especially at bonds involving basic amino acids, leucine, or glycine), yielding peptides of lower molecular weight. ␣-Galactosidase Hydrolysis of terminal nonreducing α-Dgalactose residues in α-D-galactosides. -Glucanase Hydrolysis of β-1,3- and β-1,4-linkages in β-Dglucans, yielding oligosaccharides and glucose. Glucoamylase (Amyloglucosidase) Hydrolysis of terminal α1,4- and α-1,6-glucan bonds in polysaccharides (starch, glycogen, etc.), yielding glucose (dextrose). Glucose Isomerase (Xylose isomerase) cose to fructose, and xylose to xylulose. Glucose Oxidase H2O2.
Isomerization of glu-
β-D-glucose + O2 → D-glucono-δ-lactone +
-D-Glucosidase Hydrolysis of terminal, nonreducing β-Dglucose residues with the release of β-D-glucose. Hemicellulase Hydrolysis of β-1,4-glucans, α-L-arabinosides, β-D-mannosides, 1,3-β-D-xylans, and other polysaccharides, yielding polysaccharides of lower molecular weight. Invertase (β-fructofuranosidase) Hydrolysis of sucrose to a mixture of glucose and fructose (invert sugar). Lactase (β-galactosidase) Hydrolysis of lactose to a mixture of glucose and galactose. Lysozyme Hydrolysis of cell-wall polysaccharides of various bacterial species leading to the breakdown of the cell wall most often in Gram-positive bacteria. Maltogenic Amylase Hydrolysis of α-1,4-glucan bonds. Lipase Hydrolysis of triglycerides of simple fatty acids, yielding mono- and diglycerides, glycerol, and free fatty acids. Pancreatin α-Amylase Hydrolysis of α-1,4-glucan bonds. Protease Hydrolysis of proteins and polypepticles. Lipase Hydrolysis of triglycerides of simple fatty acids.
-Amylase Hydrolysis of α-1,4-glucan bonds in polysaccharides (starch, glycogen, etc.), yielding maltose and β-limit dextrins.
Pectinase Pectate lyase Hydrolysis of pectate to oligosaccharides. Pectin depolymerase Hydrolysis of 1,4-galacturonide bonds. Pectin lyase Hydrolysis of oligosaccharides formed by pectate lyase. Pectinesterase Demethylation of pectin.
Bromelain Hydrolysis of polypeptides, amides, and esters (especially at bonds involving basic amino acids, leucine, or glycine), yielding peptides of lower molecular weight.
Pepsin Hydrolysis of polypeptides, including those with bonds adjacent to aromatic or dicarboxylic L-amino acid residues, yielding peptides of lower molecular weight.
␣-Amylase Endohydrolysis of α-1,4-glucan bonds in polysaccharides (starch, glycogen, etc.), yielding dextrins and oligoand monosaccharides.
Catalase
2H2O2 → O2 + 2H2O.
Phospholipase A2 Hydrolysis of lecithins and phosphatidylcholine, producing fatty acid anions.
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Phytase 3-Phytase myo-Inositol hexakisphosphate + H 2O → 1,2,4,5,6-pentakisphosphate + orthophosphate Acid Phosphatase Orthophosphate monoester + H2O → an alcohol + orthophosphate. Protease (generic) Hydrolysis of polypeptides, yielding peptides of lower molecular weight. Pullulanase Hydrolysis of 1,6-α-D-glycosidic bonds on amylopectin and glycogen and in α- and β-limit dextrins, yielding linear polysaccharides. Rennet (Bovine and calf) Hydrolysis of polypeptides; specificity may be similar to pepsin. Trypsin Hydrolysis of polypeptides, amides, and esters at bonds involving the carboxyl groups of L-arginine and L-lysine, yielding peptides of lower molecular weight. GENERAL REQUIREMENTS Enzyme preparations are produced in accordance with good manufacturing practices. Regardless of the source of derivation, they should cause no increase in the total microbial count in the treated food over the level accepted for the respective food. Animal tissues used to produce enzymes must comply with the applicable U.S. meat inspection requirements and must be handled in accordance with good hygienic practices. Plant material used to produce enzymes or culture media used to grow microorganisms consist of components that leave no residues harmful to health in the finished food under normal conditions of use. Preparations derived from microbial sources are produced by methods and under culture conditions that ensure a controlled fermentation, thus preventing the introduction of microorganisms that could be the source of toxic materials and other undesirable substances. The carriers, diluents, and processing aids used to produce the enzyme preparations shall be substances that are acceptable for general use in foods, including water and substances that are insoluble in foods but removed from the foods after processing. Although limits have not been established for mycotoxins, appropriate measures should be taken to ensure that the products do not contain such contaminants.
FCC IV, Supplement 3
declared representations for enzyme activity:1 Acid Phosphatase Activity, α-Amylase Activity (Nonbacterial); Bacterial α-Amylase Activity (BAU); Catalase Activity; Cellulase Activity; Chymotrypsin Activity; Diastase Activity (Diastatic Power); α-Galactosidase Activity, β-Glucanase Activity; Glucoamylase Activity (Amyloglucosidase Activity); Glucose Isomerase Activity; Glucose Oxidase Activity; β-D-Glucosidase Activity; Hemicellulase Activity; Invertase Activity; Lactase (Neutral) (β-Galactosidase) Activity; Lactase (Acid) (β-Galactosidase) Activity; Lipase Activity; Lipase/Esterase (Forestomach) Activity; Maltogenic Amylase Activity; Milk-Clotting Activity; Pancreatin Activity; Pepsin Activity; Phospholipase Activity; Phytase Activity; Plant Proteolytic Activity; Proteolytic Activity, Bacterial (PC); Proteolytic Activity, Fungal (HUT); Proteolytic Activity, Fungal (SAP); Pullulanase Activity; and Trypsin Activity. Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 5 µg of lead ion (Pb) in the control. Microbial Limits: Coliforms Proceed as directed in chapter 4 of the FDA Bacteriological Analytical Manual, Eighth Edition, 1998. Salmonella sp. Proceed as directed in chapter 5 of the FDA Bacteriological Analytical Manual, Eighth Edition, 1998. Packaging and Storage Store in tight containers in a cool, dry place.
ADDITIONAL REQUIREMENTS Assay Not less than 85.0% and not more than 115.0% of the declared units of enzyme activity. Lead Not more than 5 mg/kg. Microbial Limits: Coliforms Not more than 30 per g. Salmonella sp. Negative in 25 g. TESTS Assay The following procedures, which are included in the General Tests under Enzyme Assays, Appendix V, are provided for application as necessary in determining compliance with the
1Because of the varied conditions under which pectinases are employed, and because laboratory hydrolysis of a purified pectin substrate does not correlate with results observed with the natural substrates under use conditions, pectinase suppliers and users should develop their own assay procedures that would relate to the specific application under consideration.
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Monographs / Ethoxyquin / 23
Revision: Description, Assay Limit, and Assay Test modified; Heavy Metals (as Pb) specification and determination deleted; Lead, p-Phenetidine, and pPhenetidine-Related Impurities specifications and determinations added.
Ethoxyquin 6-Ethoxy-1,2-dihydro-2,2,4-trimethylquinoline CH3 C2H5O N H
C14H19NO
CH3 CH3
Formula wt, monomer 217.31
INS: 324
CAS: [91-53-2]
DESCRIPTION Ethoxyquin occurs as a clear yellow to red liquid that may darken with age without affecting its antioxidant activity. It is a mixture consisting predominantly of the monomer (C14H19NO). It also contains dimers and other polymers of C14H19NO. Its specific gravity is about 1.02, and its refractive index is about 1.57. Functional Use in Foods
Antioxidant.
REQUIREMENTS Identification A solution of 1 mg of sample in 10 mL of acetonitrile exhibits a strong fluorescence when viewed under short-wavelength ultraviolet light. Assay Not less than 91.0% of C14H19NO. Lead Not more than 2 mg/kg. p-Phenetidine Not more than 3.0%. p-Phenetidine-Related Impurities (low-boiling monomers and high-boiling dimers, trimers, and oligomers of Ethoxyquin) Not more than 8.0%. TESTS Assay Transfer about 200 mg of sample, accurately weighed, into a 150-mL beaker containing 50 mL of glacial acetic acid, and immediately titrate with 0.1 N perchloric acid in glacial acetic acid, determining the endpoint potentiometrically. Perform a blank determination and make any necessary correction (see General Provisions). Each mL of 0.1 N perchloric acid is equivalent to 21.73 mg of C14H19NO. Lead Determine as directed for Flame Atomic Absorption Spectrophotometric Method under the Lead Limit Test, Appendix IIIB, using a 10-g sample. p-Phenetidine Standard Preparation Transfer 6 mg of 98% p-phenetidine, available from Aldrich Chemical Co., accurately weighed,
into a 50-mL volumetric flask. Dissolve in n-hexane, dilute to volume with the same solvent, and mix. Sample Preparation Transfer 500 mg of sample, accurately weighed, into a 25-mL volumetric flask, dissolve in nhexane, dilute to volume, and mix. Procedure Inject 1-µL aliquots of the Standard Preparation and the Sample Preparation into a gas chromatograph equipped with a split injector, a flame-ionization detector, and a 25-m fused silica capillary column coated with a 2-µm film of 7% cyanopropyl-7% phenyl-85% methyl-1% vinylpolysiloxane (CPSil 19 CB, Chrompack Middelburg, or equivalent). Maintain the column at 100°, raising the temperature at 8°/min to a final temperature of 300°. Set the injector temperature to 270°and the detector temperature to 270°. Use a mixture of helium and methane, at a split ratio of 1:100, as the carrier gas, flowing at 120 mL/ min. Run the chromatogram for 27 min. Calculate the quantity, in %, of p-phenetidine in the sample taken by the formula 100 × [25C × (rU/rS)/W], in which C is the concentration, in mg/mL, of p-phenetidine in the Standard Preparation, rU is the p-phenetidine peak area response from the Sample Preparation, rS is the peak area response of pphenetidine from the Standard Preparation eluting at about 7 min, and W is the weight, in mg, of sample in the Sample Preparation. p-Phenetidine-Related Impurities Calculate the quantity, in %, of related impurities by the formula 100 – (% Assay + % p-phenetidine). Packaging and Storage Store in tightly closed carbon steel or black iron (not rubber, neoprene, or nylon) containers or in polypropylene or polyethylene drums or lined drums in a cool, dark place. Prolonged exposure to sunlight causes polymerization.
24 / FD&C Blue No. 1 / Monographs
FCC IV, Supplement 3
Revision: Entire monograph rewritten to reflect U.S. FDA regulations regarding certified FD&C color additives. The noncertified color additive, commonly referred to as Brilliant Blue FCF, is not permitted for use in food in the United States.
FD&C Blue No. 11 Brilliant Blue FCF;2 CI 42090;2 Class: Triphenylmethane C2H5
SO3Na
TESTS
SO3Na
FDA-certifiable color additives are batch certified by the United States Food and Drug Administration using analytical chemistry methods developed for this purpose by the FDA. The color additive regulations are described in Title 21, Parts 70 to 82, of the United States Code of Federal Regulations (21 CFR Parts 70 to 82). The batch certification process is described in 21 CFR Part 80. Current certification analytical methods are available from the Office of Cosmetics and Colors, Colors Certification Branch (HFS-107), U.S. Food and Drug Administration, 200 C Street, S.W., Washington, DC 20204.
N CH2 C SO3
N CH2 C2H5
C37H34N2O9S3Na2
Formula wt 792.86
INS: 133
CAS: [3844-45-9]
DESCRIPTION
Packaging and Storage
FD&C Blue No. 1 is principally the disodium salt of ethyl[4-[p[ethyl(m-sulfobenzyl)amino]-α-(o-sulfophenyl)benzylidene]2,5-cyclohexadien-1-ylidene](m-sulfobenzyl) ammonium hydroxide inner salt, with smaller amounts of the isomeric disodium salts of ethyl[4-[p-[ethyl(p-sulfobenzyl)amino]-α-(o-sulfophenyl)benzylidene]-2,5-cyclohexadien-1-ylidene](p-sulfobenzyl) ammonium hydroxide inner salt and ethyl[4-[p-[ethyl(o-sulfobenzyl)amino]-α-(o-sulfophenyl)benzylidene]-2,5-cyclohexadien-1-ylidene](o-sulfobenzyl) ammonium hydroxide inner salt. Functional Use in Foods
Total Color Not less than 85.0%. Uncombined Intermediates and Products of Side Reactions o-, m-, and p-Sulfobenzaldehydes Not more than 1.5%, combined. N-Ethyl, N-(m-sulfobenzyl)sulfanilic Acid Not more than 0.3%. Volatile Matter (at 135°) and Chlorides and Sulfates (as sodium salts) Not more than 15.0% in combination. Water-Insoluble Matter Not more than 0.2%.
Color.
Store in well-closed containers.
Revision: Entire monograph revised to reflect U.S. FDA regulations regarding certified FD&C color additives. The noncertified color additive, commonly referred to as Indigotine, is not permitted for use in food in the United States.
FD&C Blue No. 21 Indigotine;2 Indigo Carmine;2 CI 73015;2 Class: Indigoid
REQUIREMENTS Identification The visible absorption spectrum of a sample of FD&C Blue No. 1 dissolved in 0.04 N aqueous ammonium acetate has a wavelength maximum of 630 nm, with an absorptivity of 0.164 L/(mg·cm). Arsenic (as As) Not more than 3 mg/kg. Chromium (as Cr) Not more than 0.005%. Manganese (as Mn) Not more than 0.01%. Ether Extracts3 (combined) Not more than 0.4%. Lead (as Pb) Not more than 10 mg/kg. Leuco Base Not more than 5%. Subsidiary Colors Not more than 6.0%.
1To be used or sold in the United States, this color additive must
be batch certified by the U.S. Food and Drug Administration. The monograph title is the name of the color additive only after batch certification has been completed. 2Generic designations; not synonyms for certified batches of color additive. 3Not required for certification in the United States.
NaO3S
O C N
H C C
H
N C O
C16H8N2O8S2Na2
SO3Na
Formula wt 466.36
INS: 132
CAS: [860-22-0]
DESCRIPTION FD&C Blue No. 2 is principally the disodium salt of 2-(1,3dihydro-3-oxo-5-sulfo-2H-indol-2-ylidene)-2,3-dihydro-3-oxo1H-indole-5-sulfonic acid, with smaller amounts of the disodium salt of 2-(1,3-dihydro-3-oxo-7-sulfo-2H-indol-2-ylidene)-2,3dihydro-3-oxo-1H-indole-5-sulfonic acid and the sodium salt of 2-(1,3-dihydro-3-oxo-2H-indol-2-ylidene)-2,3-dihydro-3-oxo1H-indole-5-sulfonic acid. Functional Use in Foods
Color.
FCC IV, Supplement 3
Monographs / FD&C Green No. 3 / 25
REQUIREMENTS Identification The visible absorption spectrum of a sample of FD&C Blue No. 2 dissolved in 0.04 N aqueous ammonium acetate has a wavelength maximum of 610 nm, with an absorptivity of 0.0478 L/(mg·cm). Arsenic (as As) Not more than 3 mg/kg. Ether Extracts3 (combined) Not more than 0.4%. Lead (as Pb) Not more than 10 mg/kg. Mercury (as Hg) Not more than 1 mg/kg. Subsidiary and Isomeric Colors Disodium Salt of 2-(1,3-Dihydro-3-oxo-7-sulfo-2H-indol2-ylidene)-2,3-dihydro-3-oxo-1H-indole-5-sulfonic Acid Not more than 18%. Sodium Salt of 2-(1,3-Dihydro-3-oxo-2H-indol-2-ylidene)2,3-dihydro-3-oxo-1H-indole-5-sulfonic Acid Not more than 2%. Total Color Not less than 85%. Decomposition Products Isatin-5-sulfonic Acid Not more than 0.4%. 5-Sulfoanthranilic Acid Not more than 0.2%. Volatile Matter (at 135°) and Chlorides and Sulfates (as sodium salts) Not more than 15% in combination. Water-Insoluble Matter Not more than 0.4%. TESTS FDA-certifiable color additives are batch certified by the United States Food and Drug Administration using analytical chemistry methods developed for this purpose by the FDA. The color additive regulations are described in Title 21, Parts 70 to 82, of the United States Code of Federal Regulations (21 CFR Parts 70 to 82). The batch certification process is described in 21 CFR Part 80. Current certification analytical methods are available from the Office of Cosmetics and Colors, Colors Certification Branch (HFS-107), U.S. Food and Drug Administration, 200 C Street, S.W., Washington, DC 20204. Packaging and Storage
Store in well-closed containers.
Revision: Entire monograph revised to reflect U.S. FDA regulations regarding certified FD&C color additives. The noncertified color additive, commonly referred to as Fast Green FCF, is not permitted for use in food in the United States.
FD&C Green No. 31 Fast Green FCF;2 CI 42053;2 Class: Triphenylmethane C2H5
SO3 HO
SO3Na
N CH2 C2H5
C
N CH2 SO3Na
C37H34N2O10S3Na2
Formula wt 808.86
INS: 143
CAS: [2353-45-9]
DESCRIPTION FD&C Green No. 3 is principally the inner salt disodium salt of Nethyl-N-[4-[[4-[ethyl[(3-sulfophenyl)methyl]amino]phenyl](4hydroxy-2-sulfophenyl)methylene]-2,5-cyclohexadien-1ylidene]-3-sulfobenzenemethanaminium hydroxide, with smaller amounts of the isomeric inner salt disodium salt of N-ethyl-N-[4[[4-[ethyl[(3-sulfophenyl)methyl]amino]phenyl](4-hydroxy-2sulfophenyl)methylene]-2,5-cyclohexadien-1-ylidene]-4-sulfobenzenemethanaminium hydroxide; of N-ethyl-N-[4-[[4-[ethyl [(4-sulfophenyl)methyl]amino]phenyl](4-hydroxy-2-sulfophenyl)methylene]-2,5-cyclohexadien-1-ylidene]-4-sulfobenzenemethanaminium hydroxide; and of N-ethyl-N-[4-[[4-[ethyl[(2sulfophenyl)methyl]amino]phenyl](4-hydroxy-2-sulfophenyl)methylene]-2,5-cyclohexadien-1-ylidene]-3-sulfobenzenemethanaminium hydroxide. Functional Use in Foods
Color.
REQUIREMENTS Identification The visible absorption spectrum of a sample of FD&C Green No. 3 dissolved in 0.04 N aqueous ammonium acetate has a wavelength maximum of 625 nm, with an absorptivity of 0.156 L/(mg·cm). Arsenic (as As) Not more than 3 mg/kg. Chromium (as Cr) Not more than 0.005%. Ether Extracts3 (combined) Not more than 0.4%. 1To be used or sold in the United States, this color additive must
be batch certified by the U.S. Food and Drug Administration. The monograph title is the name of the color additive only after batch certification has been completed. 2Generic designations; not synonyms for certified batches of color additive. 3Not required for certification in the United States.
26 / FD&C Red No. 3 / Monographs
Lead (as Pb) Not more than 10 mg/kg. Leuco Base Not more than 5%. Mercury (as Hg) Not more than 1 mg/kg. Subsidiary Colors Not more than 6%. Total Color Not less than 85%. Uncombined Intermediates and Products of Side Reactions Sum of 3- and 4-[[Ethyl(4-sulfophenyl)amino]methyl]benzenesulfonic Acid, Disodium Salts Not more than 0.3%. Sum of 2-, 3-, and 4-Formylbenzenesulfonic Acids, Sodium Salts Not more than 0.5%. 2-Formyl-5-hydroxybenzenesulfonic Acid, Sodium Salt Not more than 0.5%. Volatile Matter (at 135°) and Chlorides and Sulfates (as sodium salts) Not more than 15.0% in combination. Water-Insoluble Matter Not more than 0.2%.
FCC IV, Supplement 3
Revision: Entire monograph revised to reflect U.S. FDA regulations regarding certified FD&C color additives. The noncertified color additive, commonly referred to as Erythrosine, is not permitted for use in food in the United States.
FD&C Red No. 31 Erythrosine;2 CI 45430;2 Class: Xanthene I NaO I
I O C
O I COONa
TESTS FDA-certifiable color additives are batch certified by the United States Food and Drug Administration using analytical chemistry methods developed for this purpose by the FDA. The color additive regulations are described in Title 21, Parts 70 to 82, of the United States Code of Federal Regulations (21 CFR Parts 70 to 82). The batch certification process is described in 21 CFR Part 80. Current certification analytical methods are available from the Office of Cosmetics and Colors, Colors Certification Branch (HFS-107), U.S. Food and Drug Administration, 200 C Street, S.W., Washington, DC 20204.
C20H6O5I4Na2
Formula wt 879.86
INS: 127
CAS: [16423-68-0]
Packaging and Storage
Functional Use in Foods
Store in well-closed containers.
DESCRIPTION FD&C Red No. 3 is principally the monohydrate of 9-(o-carboxyphenyl)-6-hydroxy-2,4,5,7-tetraiodo-3H-xanthen-3-one disodium salt, with smaller amounts of lower iodinated fluoresceins. Color.
REQUIREMENTS Identification The visible absorption spectrum of a sample of FD&C Red No. 3 dissolved in 0.05% aqueous ammonium hydroxide has a wavelength maximum of 527 nm, with an absorptivity of 0.110 L/(mg·cm). Arsenic (as As) Not more than 3 mg/kg. Ether Extracts3 (combined) Not more than 0.2%. Lead (as Pb) Not more than 10 mg/kg. Subsidiary Colors Monoiodofluoresceins Not more than 1.0%. Other Lower Iodinated Fluoresceins Not more than 9.0%. Total Color Not less than 87.0%. Uncombined Intermediates and Products of Side Reactions 2-(2',4'-Dihydroxy-3',5'-diiodobenzoyl)benzoic Acid Not more than 0.2%. Sodium Iodide Not more than 0.4%. Triiodoresorcinol Not more than 0.2%. Unhalogenated Intermediates, Total Not more than 0.1%. 1To be used or sold in the United States, this color additive must
be batch certified by the U.S. Food and Drug Administration. The monograph title is the name of the color additive only after batch certification has been completed. 2Generic designations; not synonyms for certified batches of color additive. 3Not required for certification in the United States.
FCC IV, Supplement 3
Monographs / FD&C Red No. 40 / 27
Volatile Matter (at 135°) and Chlorides and Sulfates (as sodium salts) Not more than 13% in combination. Water-Insoluble Matter Not more than 0.2%. TESTS FDA-certifiable color additives are batch certified by the United States Food and Drug Administration using analytical chemistry methods developed for this purpose by the FDA. The color additive regulations are described in Title 21, Parts 70 to 82, of the United States Code of Federal Regulations (21 CFR Parts 70 to 82). The batch certification process is described in 21 CFR Part 80. Current certification analytical methods are available from the Office of Cosmetics and Colors, Colors Certification Branch (HFS-107), U.S. Food and Drug Administration, 200 C Street, S.W., Washington, DC 20204. Packaging and Storage
Store in well-closed containers.
Revision: Entire monograph revised to reflect U.S. FDA regulations regarding certified FD&C color additives. The noncertified color additive, commonly referred to as Allura Red AC, is not permitted for use in food in the United States.
FD&C Red No. 401 Allura
Red AC;2
CI
16035;2
REQUIREMENTS Identification The visible absorption spectrum of a sample of FD&C Red No. 40 dissolved in 0.04 N aqueous ammonium acetate has a wavelength maximum of 500 nm, with an absorptivity of 0.052 L/(mg·cm). Arsenic (as As) Not more than 3 mg/kg. Lead (as Pb) Not more than 10 mg/kg. Subsidiary Colors Disodium Salt of 6-Hydroxy-5-[(2-methoxy-5-methyl-4sulfophenyl)azo]-8-(2-methoxy-5-methyl-4-sulfophenoxy)-2naphthalenesulfonic Acid Not more than 1.0%. Higher Sulfonated Subsidiary Colors (as sodium salts) Not more than 1.0%. Lower Sulfonated Subsidiary Colors (as sodium salts) Not more than 1.0%. Total Color Not less than 85.0%. Uncombined Intermediates and Products of Side Reactions 4-Amino-5-methoxy-o-toluenesulfonic Acid Not more than 0.2%. Disodium Salt of 6,6'-Oxybis(2-naphthalenesulfonic Acid) Not more than 1.0%. Sodium Salt of 6-Hydroxy-2-naphthalenesulfonic Acid Not more than 0.3%. Volatile Matter (at 135°) and Chlorides and Sulfates (as sodium salts) Not more than 14.0% in combination. Water-Insoluble Matter Not more than 0.2%. TESTS
Class: Monoazo CH3
OH
SO3Na
N N OCH3 SO3Na
C18H14N2O8S2Na2
Formula wt 496.43
INS: 129
CAS: [25956-17-6]
FDA-certifiable color additives are batch certified by the United States Food and Drug Administration using analytical chemistry methods developed for this purpose by the FDA. The color additive regulations are described in Title 21, Parts 70 to 82, of the United States Code of Federal Regulations (21 CFR Parts 70 to 82). The batch certification process is described in 21 CFR Part 80. Current certification analytical methods are available from the Office of Cosmetics and Colors, Colors Certification Branch (HFS-107), U.S. Food and Drug Administration, 200 C Street, S.W., Washington, DC 20204. Packaging and Storage
DESCRIPTION FD&C Red No. 40 is principally the disodium salt of 6-hydroxy5-[(2-methoxy-5-methyl-4-sulfophenyl)azo]-2-naphthalenesulfonic acid. Functional Use in Foods
Color.
1To be used or sold in the United States, this color additive must
be batch certified by the U.S. Food and Drug Administration. The monograph title is the name of the color additive only after batch certification has been completed. 2Generic designations; not synonyms for certified batches of color additive.
Store in well-closed containers.
28 / FD&C Yellow No. 5 / Monographs
FCC IV, Supplement 3
Revision: Entire monograph revised to reflect U.S. FDA regulations regarding certified FD&C color additives. The noncertified color additive, commonly referred to as Tartrazine, is not permitted for use in food in the United States.
FD&C Yellow No. 51 Tartrazine;2 CI 19140;2 Class: Pyrazolone NaO3S
N N C
C COONa N
HO C N
SO3Na
C16H9N4O9S2Na3
Formula wt 534.37
INS: 102
CAS: [1934-21-0]
Ethyl or Methyl 4,5-Dihydro-5-oxo-1-(4-sulfophenyl)-4-[(4sulfophenyl)hydrazono]-1H-pyrazole-3-carboxylate, Disodium Salt Not more than 1%. Sum of 4,5-Dihydro-5-oxo-1-phenyl-4-[(4-sulfophenyl)azo]1H-pyrazole-3-carboxylic Acid, Disodium Salt, and 4,5-Dihydro5-oxo-4-(phenylazo)-1-(4-sulfophenyl)-1H-pyrazole-3-carboxylic Acid, Disodium Salt Not more than 0.5%. 4-Aminobenzenesulfonic Acid, Sodium Salt Not more than 0.2%. 4,5-Dihydro-5-oxo-1-(4-sulfophenyl)-1H-pyrazole-3-carboxylic Acid, Disodium Salt Not more than 0.2%. Ethyl or Methyl 4,5-Dihydro-5-oxo-1-(4-sulfophenyl)-1Hpyrazole-3-carboxylate, Sodium Salt Not more than 0.1%. 4,4'-(1-Triazene-1,3-diyl)bis[benzenesulfonic acid], Disodium Salt Not more than 0.05%. 4-Aminoazobenzene Not more than 75 µg/kg. 4-Aminobiphenyl Not more than 5 µg/kg. Aniline Not more than 100 µg/kg. Azobenzene Not more than 40 µg/kg. Benzidine Not more than 1 µg/kg. 1,3-Diphenyltriazene Not more than 40 µg/kg. Volatile Matter (at 135°) and Chlorides and Sulfates (as sodium salts) Not more than 13% in combination. Water-Insoluble Matter Not more than 0.2%.
DESCRIPTION FD&C Yellow No. 5 is principally the trisodium salt of 4,5dihydro-5-oxo-1-(4-sulfophenyl)-4-[4-sulfophenyl-azo]-1Hpyrazole-3-carboxylic acid. Functional Use in Foods
Color.
REQUIREMENTS Identification The visible absorption spectrum of a sample of FD&C Yellow No. 5 dissolved in 0.04 N aqueous ammonium acetate has a wavelength maximum of 428 nm, with an absorptivity of 0.053 L/(mg·cm). Arsenic (as As) Not more than 3 mg/kg. Ether Extracts3 (combined) Not more than 0.2%. Lead (as Pb) Not more than 10 mg/kg. Mercury (as Hg) Not more than 1 mg/kg. Total Color Not less than 87%. Uncombined Intermediates and Products of Side Reactions 4,4'-[4,5-Dihydro-5-oxo-4-[(4-sulfophenyl)-hydrazono]1H-pyrazol-1,3-diyl]bis[benzenesulfonic Acid], Trisodium Salt Not more than 1%. 4-[(4',5-Disulfo[1,1'-biphenyl]-2-yl)hydrazono]-4,5dihydro-5-oxo-1-(4-sulfophenyl)-1H-pyrazole-3-carboxylic Acid, Tetrasodium Salt Not more than 1%.
1To be used or sold in the United States, this color additive must
be batch certified by the U.S. Food and Drug Administration. The monograph title is the name of the color additive only after batch certification has been completed. 2Generic designations; not synonyms for certified batches of color additive. 3Not required for certification in the United States.
TESTS FDA-certifiable color additives are batch certified by the United States Food and Drug Administration using analytical chemistry methods developed for this purpose by the FDA. The color additive regulations are described in Title 21, Parts 70 to 82, of the United States Code of Federal Regulations (21 CFR Parts 70 to 82). The batch certification process is described in 21 CFR Part 80. Current certification analytical methods are available from the Office of Cosmetics and Colors, Colors Certification Branch (HFS-107), U.S. Food and Drug Administration, 200 C Street, S.W., Washington, DC 20204. Packaging and Storage
Store in well-closed containers.
FCC IV, Supplement 3
Monographs / Grape Skin Extract / 29
Revision: Entire monograph revised to reflect U.S. FDA regulations regarding certified FD&C color additives. The noncertified color additive, commonly referred to as Sunset Yellow FCF, is not permitted for use in food in the United States.
FD&C Yellow No. 61 Sunset Yellow FCF;2 CI 15985;2 Class: Monoazo OH NaO3S
N N
SO3Na
C16H10N2O7S2Na2
Formula wt 452.37
INS: 110
CAS: [2783-94-0]
DESCRIPTION FD&C Yellow No. 6 is principally the disodium salt of 6-hydroxy5-[(4-sulfophenyl)azo]-2-naphthalenesulfonic acid. The trisodium salt of 3-hydroxy-4-[(4-sulfophenyl)azo]-2,7-naphthalenedisulfonic acid may be added in small amounts. Functional Use in Foods
Sodium Salt of 4-Aminobenzenesulfonic Acid Not more than 0.2%. Sodium Salt of 6-Hydroxy-2-naphthalenesulfonic Acid Not more than 0.3%. Disodium Salt of 6,6'-Oxybis[2-naphthalenesulfonic Acid] Not more than 1%. Disodium Salt of 4,4'-(1-Triazene-1,3-diyl)bis[benzenesulfonic Acid] Not more than 0.1%. Sum of the Sodium Salt of 6-Hydroxy-5-(phenylazo)-2-naphthalenesulfonic Acid and the Sodium Salt of 4-[(2-Hydroxy-1naphthalenyl)azo]benzenesulfonic Acid Not more than 1%. Sum of the Trisodium Salt of 3-Hydroxy-4-[(4-sulfophenyl)azo]-2,7-naphthalenedisulfonic Acid and Other Higher Sulfonated Subsidiaries Not more than 5%. Volatile Matter (at 135°) and Chlorides and Sulfates (as sodium salts) Not more than 13% in combination. Water-Insoluble Matter Not more than 0.2%.
Color.
REQUIREMENTS Identification The visible absorption spectrum of a sample of FD&C Yellow No. 6 dissolved in 0.04 N aqueous ammonium acetate has a wavelength maximum of 484 nm, with an absorptivity of 0.054 L/(mg·cm). Arsenic (as As) Not more than 3 mg/kg. Ether Extracts3 (combined) Not more than 0.2%. Lead (as Pb) Not more than 10 mg/kg. Mercury (as Hg) Not more than 1 mg/kg. Total Color Not less than 87%. Uncombined Intermediates and Products of Side Reactions 4-Aminoazobenzene Not more than 50 µg/kg. 4-Aminobiphenyl Not more than 15 µg/kg. Aniline Not more than 250 µg/kg. Azobenzene Not more than 200 µg/kg. Benzidine Not more than 1 µg/kg. 1,3-Diphenyltriazene Not more than 40 µg/kg. 1-(Phenylazo)-2-naphthalenol Not more than 10 mg/kg.
1To be used or sold in the United States, this color additive must
be batch certified by the U.S. Food and Drug Administration. The monograph title is the name of the color additive only after batch certification has been completed. 2Generic designations; not synonyms for certified batches of color additive. 3Not required for certification in the United States.
TESTS FDA-certifiable color additives are batch certified by the United States Food and Drug Administration using analytical chemistry methods developed for this purpose by the FDA. The color additive regulations are described in Title 21, Parts 70 to 82, of the United States Code of Federal Regulations (21 CFR Parts 70 to 82). The batch certification process is described in 21 CFR Part 80. Current certification analytical methods are available from the Office of Cosmetics and Colors, Colors Certification Branch (HFS-107), U.S. Food and Drug Administration, 200 C Street, S.W., Washington, DC 20204. Packaging and Storage
Store in well-closed containers.
Revision: Assay and Lead specification corrected; Arsenic and Pesticides specifications and determinations deleted.
Grape Skin Extract Enocianina CAS: [11029-12-2]
DESCRIPTION Grape Skin Extract occurs as a red to purple powder or liquid concentrate. It is prepared by aqueous extraction of grape marc remaining from the pressing of grapes to obtain juice. Extraction is effected with water containing sulfur dioxide. After concentration by vacuum evaporation, the sugar content is reduced by fermentation; further concentration removes most of the alcohol. The primary color components are anthocyanins such as the glucosides of malvidin, peonidin, petunidin, delphinidin, or cyanidin. Other components naturally present are sugars, tartrates, malates, tannins, and minerals. Alcohol or sulfur dioxide may be added. The powder may contain an added carrier such as
30 /
DL-Isoleucine
/ Monographs
maltodextrin, modified starch, or gum. In acid solution, Grape Skin Extract is red; in neutral to alkaline solution, it is violet to blue. Functional Use in Foods
Color.
FCC IV, Supplement 3
Revision: Identification test corrected; Heavy Metals (as Pb) specification and determination deleted. DL-Isoleucine DL-2-Amino-3-methylvaleric Acid
REQUIREMENTS Identification Transfer 1 g of sample and 1 g of potassium metabisulfite to a 100-mL volumetric flask, dissolve in about 50 mL of pH 3.0 Citrate–Citric Acid Buffer (see Assay, below), and dilute to volume with the same buffer. The red color due to anthocyanins is bleached. Assay The color strength (CS) expressed as the absorbance of a 1% solution in pH 3.0 Citrate–Citric Acid Buffer in a cell of 1-cm pathlength shall not be less than 90% of the color strength as represented by the vendor. Lead Not more than 5 mg/kg. TESTS Assay pH 3.0 Citrate–Citric Acid Buffer Add 0.1 M sodium citrate, dropwise, to 0.1 M citric acid until a pH of 3.0 is reached, as determined by a glass electrode. Procedure Transfer about 0.2 g of sample, accurately weighed, to a 100-mL volumetric flask, dissolve in about 25 mL of pH 3.0 Citrate–Citric Acid Buffer, and dilute to volume with the same buffer. Remove any undissolved material by filtration or centrifugation. Adjust the pH to 3.0, and determine the absorbance of the clarified solution at 525 nm in a cell with a 1-cm pathlength. The color strength expressed as the absorbance of a 1% solution in a cell of 1-cm pathlength is calculated as CS = absorbance at 525 nm/sample weight in g. Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Packaging and Storage Store liquid Grape Skin Extract with aseptic packaging or in high-density polyethylene containers at 4° to 14°. Store powdered Grape Skin Extract in fiber drums at room temperature.
H3C H H3C
C6H13NO2
O
OH H NH2
Formula wt 131.17 CAS: [443-79-8]
DESCRIPTION A white, crystalline powder. It is soluble in water, but is practically insoluble in alcohol and in ether. It melts with decomposition at about 292°. The pH of a 1:100 solution is between 5.5 and 7.0. It is optically inactive. Functional Use in Foods
Nutrient; dietary supplement.
REQUIREMENTS Identification Heat 5 mL of a 1:1000 solution with 1 mL of triketohydrindene hydrate TS (ninhydrin TS). A bluish purple color is produced. Assay Not less than 98.5% and not more than 101.5% of C6H13NO2, calculated on the dried basis. Lead Not more than 10 mg/kg. Loss on Drying Not more than 0.3%. Residue on Ignition Not more than 0.1%. TESTS Assay Dissolve about 250 mg, accurately weighed, in 3 mL of formic acid and 50 mL of glacial acetic acid, add 2 drops of crystal violet TS, and titrate with 0.1 N perchloric acid to the first appearance of a pure green color or until the blue color disappears completely. Perform a blank determination (see General Provisions), and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 13.12 mg of C6H13NO2. Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Loss on Drying, Appendix IIC Dry at 105° for 3 h. Residue on Ignition, Appendix IIC Ignite 1 g as directed in the general method. Packaging and Storage
Store in well-closed containers.
FCC IV, Supplement 3
Monographs / Lanolin, Anhydrous / 31
Revision: Identification test corrected; Heavy Metals (as Pb) specification and determination deleted.
Revision: Arsenic and Heavy Metals (as Pb) specifications and determinations deleted.
L-Isoleucine
Lanolin, Anhydrous
L-2-Amino-3-methylvaleric Acid
Wool Fat
H3C H H3C
C6H13NO2
O
INS: 913
OH H NH2
Formula wt 131.17 CAS: [73-32-5]
DESCRIPTION Crystalline leaflets or a white, crystalline powder. It is soluble in 25 parts of water, slightly soluble in hot alcohol, and soluble in diluted mineral acids and in alkaline solutions. It sublimes between 168° and 170°, and melts with decomposition at about 284°. The pH of a 1:100 solution is between 5.5 and 7.0. Functional Use in Foods
Nutrient; dietary supplement.
REQUIREMENTS Identification Heat 5 mL of a 1:1000 solution with 1 mL of triketohydrindene hydrate TS (ninhydrin TS). A reddish purple or bluish purple color is produced. Assay Not less than 98.5% and not more than 101.5% of C6H13NO2, calculated on the dried basis. Lead Not more than 10 mg/kg. Loss on Drying Not more than 0.3%. Residue on Ignition Not more than 0.2%. Specific Rotation [α]20° D : Between +38.6° and +41.5° after drying; or [α]25° D : Between +38.2° and +41.1° after drying. TESTS Assay Dissolve about 250 mg, accurately weighed, in 3 mL of formic acid and 50 mL of glacial acetic acid, add 2 drops of crystal violet TS, and titrate with 0.1 N perchloric acid to the first appearance of a pure green color or until the blue color disappears completely. Perform a blank determination (see General Provisions), and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 13.12 mg of C6H13NO2. Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Loss on Drying, Appendix IIC Dry at 105° for 3 h. Residue on Ignition, Appendix IIC Ignite 1 g as directed in the general method. Specific Rotation, Appendix IIB Determine in a solution containing 4 g of a previously dried sample in sufficient 6 N hydrochloric acid to make 100 mL. Packaging and Storage
Store in well-closed containers.
DESCRIPTION A purified, yellowish white, semisolid, fatlike substance extracted from the wool of sheep. It is insoluble in water, but mixes with about twice its weight of water without separation. It is soluble in chloroform and in ether. Functional Use in Foods gum base.
Masticatory substance in chewing
REQUIREMENTS Acid Value Not more than 1.12. Iodine Value Between 18 and 36. Lead Not more than 3 mg/kg. Loss on Heating Not more than 0.5%. Melting Range Between 36° and 42°. TESTS Acid Value Determine as directed for Acid Value, Method I, under Fats and Related Substances, Appendix VII. Iodine Value Determine by the Modified Wijs Method, Appendix VII. Lead Prepare a Sample Solution as directed in the general method under Chewing Gum Base, Appendix IV. This solution meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Loss on Heating Heat a 5-g sample on a steam bath, with frequent stirring, to constant weight. Melting Range Determine as directed for Melting Range or Temperature, Appendix IIB. Packaging and Storage Store in well-closed containers, preferably at a temperature not exceeding 30°.
32 / Lemongrass Oil / Monographs
Revision: Angular Rotation changed to reflect commercial standards; Heavy Metals (as Pb) specification and determination deleted.
Lemongrass Oil
FCC IV, Supplement 3
until the addition product dissolves, and then continue the heating and intermittent shaking for another 30 min. When the liquids have separated completely, add enough of the sodium bisulfite solution to raise the lower level of the oily layer within the graduated portion of the neck of the flask. Calculate the percentage, by volume, of the citral by the formula 100 – (V × 10),
DESCRIPTION A volatile oil prepared by steam distillation of freshly cut and partially dried cymbopogon grasses indigenous to tropical and subtropical areas. Two types of Lemongrass Oil are commercially available. The East Indian type, also known as Cochin, Native, and British Indian Lemongrass Oil, is usually a dark yellow to light brownish red liquid having a pronounced heavy lemonlike odor. The West Indian type, also known as Madagascar, Guatemala, or other country of origin Lemongrass Oil, is light yellow to light brown in color and has a lemonlike odor of a lighter character than the East Indian type oil. Lemongrass Oils are soluble in mineral oil, freely soluble in propylene glycol, but practically insoluble in water and in glycerin. The East Indian variety dissolves readily in alcohol, but the West Indian oil yields cloudy solutions. Functional Use in Foods
Flavoring agent.
in which V is the number of mL of separated oil in the graduated neck of the cassia flask. Angular Rotation Determine in a 100-mm tube as directed under Optical Rotation, Appendix IIB. Refractive Index, Appendix IIB Determine with an Abbé or other refractometer of equal or greater accuracy. Solubility in Alcohol Proceed as directed in the general method, Appendix VI. East Indian type: 1 mL dissolves in 3 mL of 70% alcohol, usually with slight turbidity; West Indian type: yields a cloudy solution with 70%, 80%, 90%, and 95% alcohol. Specific Gravity Determine by any reliable method (see General Provisions). Steam-Volatile Oil Proceed as directed for Volatile Oil Content under Essential Oils and Flavors, Appendix VI, using 25.0 mL of the oil prepared as directed in the Assay. Packaging and Storage Store in a cool place in full, tight, preferably glass, aluminum, tin-lined, or other suitably lined containers, or in black iron unlined drums. If stored in glass containers, avoid exposure to light.
REQUIREMENTS Labeling Indicate whether it is the East Indian or West Indian type. Identification The infrared absorption spectrum of the sample exhibits relative maxima (that may vary in intensity) at the same wavelengths (or frequencies) as those shown in the respective spectrum under Infrared Spectra, using the same test conditions as specified therein. Assay Not less than 75.0%, by volume, of aldehydes as citral. Angular Rotation Between –10° and 0°. Refractive Index Between 1.483 and 1.489. Solubility in Alcohol Passes test. Specific Gravity East Indian type: between 0.894 and 0.904; West Indian type: between 0.869 and 0.894. Steam-Volatile Oil Not less than 93.0%, by volume.
Revision: Identification test corrected; Heavy Metals (as Pb) specification and determination deleted. DL-Leucine DL-2-Amino-4-methylvaleric Acid
O H3C H3C
C6H13NO2
OH H NH2
Formula wt 131.17 CAS: [328-39-2]
TESTS Assay Mix 50.0 mL of the sample with 500 mg of tartaric acid, shake for 5 min, and filter. Dry the filtered oil over anhydrous sodium sulfate, and then pipet 10.0 mL of the clear, treated oil into a 150-mL cassia flask. Note: Retain the remaining oil for the Steam-Volatile Oil test. Add 75 mL of a 30% solution of sodium bisulfite, stopper the flask, and shake until a semisolid to solid sodium bisulfite addition product has formed. Allow the mixture to stand at room temperature for 5 min, then loosen the stopper, and immerse the flask in a water bath heated to between 85° and 90°. Maintain the water bath at this temperature, shaking the flask occasionally,
DESCRIPTION Small, white crystals or a crystalline powder. It is freely soluble in water, slightly soluble in alcohol, and insoluble in ether. It melts with decomposition at about 290°. The pH of a 1:100 solution is between 5.5 and 7.0. It is optically inactive. Functional Use in Foods
Nutrient; dietary supplement.
REQUIREMENTS Identification Heat 5 mL of a 1:1000 solution with 1 mL of triketohydrindene hydrate TS (ninhydrin TS). A reddish purple or bluish purple color is produced.
FCC IV, Supplement 3
Monographs / Maltitol / 33
Assay Not less than 98.5% and not more than 101.5% of C6N13NO2, calculated on the dried basis. Lead Not more than 10 mg/kg. Loss on Drying Not more than 0.3%. Residue on Ignition Not more than 0.1%. TESTS Assay Dissolve about 400 mg, accurately weighed, in 3 mL of formic acid and 50 mL of glacial acetic acid. Add 2 drops of crystal violet TS, and titrate with 0.1 N perchloric acid to the first appearance of a pure green color or until the blue color disappears completely. Perform a blank determination (see General Provisions), and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 13.12 mg of C6H13NO2. Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Loss on Drying, Appendix IIC Dry at 105° for 3 h. Residue on Ignition, Appendix IIC Ignite 1 g as directed in the general method. Packaging and Storage
Store in well-closed containers.
Revision: Solubility in Alcohol and Specific Gravity changed to reflect commercial standards; Heavy Metals (as Pb) specification and determination deleted.
Lovage Oil
Saponification Value Between 238 and 258. Solubility in Alcohol Passes test. Specific Gravity Between 1.030 and 1.057. TESTS Acid Value Determine as directed for Acid Value under Essential Oils and Flavors, Appendix VI. Angular Rotation Determine in a 100-mm tube as directed under Optical (Specific) Rotation, Appendix IIB. Refractive Index, Appendix IIB Determine with an Abbé or other refractometer of equal or greater accuracy. Saponification Value Determine as directed for Saponification Value under Essential Oils and Flavors, Appendix VI, using 1.5 g accurately weighed. Solubility in Alcohol Proceed as directed in the general method, Appendix VI. One mL dissolves in 4 mL of 95% ethanol, sometimes with slight turbidity. The age of the oil has an adverse effect upon solubility. Specific Gravity Determine by any reliable method (see General Provisions). Packaging and Storage Store in full, tight, glass, aluminum, tin-lined, or other suitably lined containers in a cool place protected from light.
Revision: Description corrected; Assay limit of Dmaltitol revised; entire Identification, Assay, and Reducing Sugars tests provided.
Maltitol D-Maltitol; Hydrogenated Maltose; α-D-Glucopyranosyl-1,4-Dglucitol
DESCRIPTION The volatile oil obtained by steam distillation of the fresh root of the plant Levisticum officinale L. Koch syn. Angelica levisticum, Baillon (Fam. Umbelliferae). It is a yellow greenish brown to deep-brown liquid having a strong characteristic aromatic odor and taste. It is soluble in most fixed oils and slightly soluble, with opalescence, in mineral oil, but it is relatively insoluble in glycerin and in propylene glycol. Note: This oil becomes darker and more viscous under the influence of air and light. Functional Use in Foods
CH2OH
CH2OH O
OH CH2OH
HO OH
O OH
C12H24O11 INS: 965
OH OH
Formula wt 344.31 CAS: [585-88-6]
Flavoring agent. DESCRIPTION
REQUIREMENTS Identification The infrared absorption spectrum of the sample exhibits relative maxima (that may vary in intensity) at the same wavelengths (or frequencies) as those shown in the respective spectrum under Infrared Spectra, using the same test conditions as specified therein. Acid Value Between 2.0 and 16.0. Angular Rotation Between –1° and –5°. Refractive Index Between 1.536 and 1.554 at 20°.
Maltitol occurs as a white, crystalline powder containing small amounts of sorbitol and related polyhydric alcohols. It is very soluble in water and slightly soluble in ethanol. Functional Use in Foods
Sweetener; humectant; stabilizer.
REQUIREMENTS Identification Prepare a mixture of n-propyl alcohol, ethyl acetate, and water (70:20:10) as the Developing Solvent. Dissolve
34 / Mentha Arvensis Oil, Partially Dementholized / Monographs
USP Maltitol Reference Standard in water to obtain a Standard Solution having a concentration of 2.5 mg/mL. Prepare the Test Solution by diluting Maltitol with water to obtain a solution containing, on the anhydrous basis, about 2.5 mg of Maltitol per mL. Apply separately 2 µL each of the Standard Solution and the Test Solution to a thin-layer chromatographic plate coated with a 0.25-mm layer of chromatographic silica gel. Allow the spots to dry, and develop the plate in a developing chamber containing the Developing Solvent until the solvent front has moved about 17 cm. Remove the plate from the chamber, mark the solvent front, and allow the solvent to evaporate. Spray the plate with sodium metaperiodate solution (1:500), air-dry for 15 min, and spray with a 1-in-50 solution of 4,4'-tetramethyldiaminodiphenylmethane in a mixture of acetone and glacial acetic acid (4:1): The principal spot obtained from the Test Solution corresponds in Rf value and color to that obtained from the Standard Solution. Assay Not less that 92.0% and not more than 100.5% of Dmaltitol as C12H24O11 calculated on the anhydrous basis. Chloride Not more than 0.005%. Lead Not more than 1 mg/kg. Nickel Not more than 2 mg/kg. Reducing Sugars Not more than 0.1% (as glucose). Residue on Ignition Not more that 0.1%. Sulfate Not more than 0.01%. Water Not more than 1.0%. TESTS Assay Mobile Phase Use degassed water. Standard Preparation Dissolve an accurately weighed quantity of USP Maltitol Reference Standard in water, and dilute quantitatively with water to obtain a solution having a known concentration of about 10.0 mg/mL. Assay Solution Transfer about 0.7 g of the sample, accurately weighed, to a 50-mL volumetric flask, dilute to volume with water, and mix. Chromatographic System Use a liquid chromatograph equipped with a refractive index detector that is maintained at a constant temperature and a 9-mm × 30-cm column packed with a strong cation-exchange resin, about 9 µm in diameter, consisting of sulfonated cross-linked styrene–divinylbenzene copolymer in the calcium form (Aminex HPX-87c, or equivalent). Maintain the column temperature at 85° ± 0.5°, and the flow rate of the Mobile Phase at about 0.5 mL/min. Chromatograph the Standard Preparation, and record the peak responses as directed under Procedure. Replicate injections show a relative standard deviation not greater than 2.0%. Procedure Separately inject suitable portions (about 20 µL) of the Assay Preparation and the Standard Preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks. The elution pattern includes the higher molecular weight hydrogenated polysaccharides, followed by three individual peaks representing maltotriitol, maltitol, and sorbitol. The principal peak is maltitol, which elutes at about twice the retention time of the void volume, and the retention time for sorbitol is about 1.7 relative to maltitol. Calculate the quantity, in mg, of D-maltitol in the portion of the sample taken by the formula
FCC IV, Supplement 3
50C × (rU/rS), in which C is the concentration, in mg/mL, of USP Maltitol Reference Standard in the Standard Preparation, and rU and rS are the peak responses of Maltitol obtained from the Assay Preparation and the Standard Preparation, respectively. Chloride Determine as directed for Chloride Test under Chloride and Sulfate Limit Tests, Appendix IIIB. Any turbidity produced by a 10.0-g sample does not exceed that shown in a control containing 1.5 mL of 0.01 N hydrochloric acid. Lead Determine as directed for Flame Atomic Absorption Spectrophotometric Method under the Lead Limit Test, Appendix IIIB, using a 10-g sample. Nickel Determine as directed under the Nickel Limit Test, Appendix IIIB, using a 20.0-g sample. Reducing Sugars Dissolve 21 g of the sample in 35 mL of water in a 400-mL beaker and mix. Add 25 mL of cupric sulfate TS and 25 mL of alkaline cupric tartrate TS. Cover the beaker with a watch glass, heat the mixture at such a rate that it comes to a boil in approximately 4 min and boils for exactly 2 min. Filter the precipitated cuprous oxide through a tared, sintered-glass filter crucible previously washed with hot water, ethanol, and ether and dried at 100° for 30 min. Thoroughly wash the collected cuprous oxide on the filter with hot water, then with 10 mL of ethanol and finally with 10 mL of ether, and dry at 100° for 30 min. The weight of the cuprous oxide does not exceed 50 mg. Residue on Ignition Determine as directed for Method I (for solids) under Residue on Ignition, Appendix IIC, igniting a 2-g sample. Sulfate Determine as directed for Sulfate Test under Chloride and Sulfate Limit Tests, Appendix IIIB. Any turbidity produced by a 10.0-g sample does not exceed that shown in a control containing 2.0 mL of 0.01 N sulfuric acid. Water Determine as directed for the Karl Fischer Titrimetric Method under Water Determination, Appendix IIB. Packaging and Storage
Store in well-closed containers.
Angular Rotation corrected to reflect commercial standards; Heavy Metals (as Pb) specification and determination deleted.
Mentha Arvensis Oil, Partially Dementholized Cornmint Oil, Partially Dementholized
DESCRIPTION The portion of oil remaining after the partial removal of menthol, by freezing operations only, from the oil of Mentha arvensis var. piperascens Holmes (forma piperascens Malinvaud). It is a colorless to yellow liquid having a characteristic minty odor. It is soluble in most fixed oils, in mineral oil, and in propylene glycol. It is insoluble in glycerin. Functional Use in Foods
Flavoring agent.
FCC IV, Supplement 3
REQUIREMENTS Identification The infrared absorption spectrum of the sample exhibits relative maxima (that may vary in intensity) at the same wavelengths (or frequencies) as those shown in the respective spectrum in the section on Infrared Spectra, using the same test conditions as specified therein. Assay Not less than 40.0% and not more than 60.0% of total alcohols, calculated as menthol (C10H20O). Angular Rotation Between –30° and –10°. Refractive Index Between 1.458 and 1.465 at 20°. Solubility in Alcohol Passes test. Specific Gravity Between 0.888 and 0.908. Total Esters Between 5.0% and 20.0%, calculated as menthyl acetate (C12H22O2). Total Ketones Between 30.0% and 50.0%, calculated as menthone (C10H18O). TESTS Assay Proceed as directed under Total Alcohols, Appendix VI, using about 1.5 g of the acetylated oil, accurately weighed, for the saponification. Calculate the percentage of alcohol, as menthol, in the sample by the formula A × 7.813(1 – 0.0021E)/(B – 0.021A), in which A is the number of mL of 0.5 N alcoholic potassium hydroxide consumed in the saponification; B is the weight, in g, of the acetylated oil taken; and E is the percentage of esters, as menthyl acetate, determined as directed under Total Esters below. Angular Rotation Determine in a 100-mm tube as directed under Optical (Specific) Rotation, Appendix IIB. Refractive Index, Appendix IIB Determine with an Abbé or other refractometer of equal or greater accuracy. Solubility in Alcohol Proceed as directed in the general method. One mL dissolves in 2.5 to 4 mL of 80% alcohol and may become hazy upon further dilution. Specific Gravity Determine by any reliable method (see General Provisions). Total Esters Weigh accurately about 10 g, and proceed as directed under Ester Determination, Appendix VI, using 99.15 as the equivalence factor (e) in the calculation. Total Ketones Weigh accurately about 1 g, and proceed as directed for ketones under Aldehydes and Ketones—Hydroxylamine Method, Appendix VI, using 77.12 as the equivalence factor (e) in the calculation. Packaging and Storage Store in full, tight containers in a cool place protected from light.
Monographs / Pectins / 35
Revision: Correction made to Degree of Amide Substitution and Total Galacturonic Acid in the Pectin Component; Heavy Metals (as Pb) specification and determination deleted.
Pectins INS: 440
CAS: [9000-69-5]
DESCRIPTION Pectins consist mainly of the partial methyl esters of polygalacturonic acid and their sodium, potassium, calcium, and ammonium salts. Pectin is obtained by extraction in an aqueous medium of appropriate edible plant material, usually citrus fruits or apples. No organic precipitants shall be used other than methanol, ethanol, and isopropanol. In some types, a portion of the methyl esters may have been converted to primary amides by treatment with ammonia under alkaline conditions. It usually occurs as a white, yellowish, light grayish, or light brownish powder. It dissolves in water, forming an opalescent, colloidal dispersion. It is practically insoluble in ethanol. The commercial product is normally diluted with sugars for standardization purposes. In addition to sugars, pectins may be mixed with suitable food-grade salts required for pH control and desirable setting characteristics. Note: The following REQUIREMENTS and TESTS apply to the Pectins as supplied, whether standardized or not, except for specifications covering amide substitution and the weight percent of total galacturonic acid in the Pectin component, in which cases the test procedures provide for removing the sugars and soluble salts before analysis of the Pectin component. Functional Use in Foods emulsifier.
Gelling agent; thickener; stabilizer;
REQUIREMENTS Labeling Indicate the presence of sulfur dioxide if the residual concentration is greater than 10 mg/kg. Identification A. To a 1:100 aqueous solution of the sample add an equal volume of alcohol. A translucent, gelatinous precipitate is formed (most gums will not form such a precipitate). B. To 5.0 mL of a 1:100 aqueous solution of the sample add 0.1 mL of a 0.125 M solution of calcium chloride or calcium acetate (equivalent to 10 mg of calcium per g of sample) and 1 mL of 1 N sodium hydroxide, and allow to stand at room temperature for 15 min. A gel or semi-gel forms (tragacanth and other gums will not form such a precipitate). C. Acidify the gel formed from Identification Test B with 1 mL of 2.7 N hydrochloric acid, and shake well. If necessary, continue adding the acid dropwise until the mixture is acid to litmus. A voluminous, colorless, gelatinous precipitate forms, which, upon boiling, becomes white and flocculent (pectic acid).
36 / Pectins / Monographs
Acid-Insoluble Ash Not more than 1.0%. Arsenic (as As) Not more than 3 mg/kg. Degree of Amide Substitution and Total Galacturonic Acid in the Pectin Component Not more than 25% of total carboxylic groups. Lead Not more than 5 mg/kg. Loss on Drying Not more than 12.0%. Methanol, Ethanol, and Isopropanol Not more than 1.0% total. Sodium Methyl Sulfate Not more than 0.1%. Sulfur Dioxide Not more than 0.005%. Total Galacturonic Acid in Pectin Component Not less than 65.0%, calculated on the ash-free, dried basis. TESTS Acid-Insoluble Ash Determine as directed in the general method, Appendix IIC. Arsenic A Sample Solution prepared as directed for organic compounds meets the requirements of the Arsenic Test, Appendix IIIB. Degree of Amide Substitution and Total Galacturonic Acid in the Pectin Component Weigh 5 g of the sample to the nearest 0.1 mg, and transfer to a suitable beaker. Stir for 10 min with a mixture of 5 mL of 2.7 N hydrochloric acid, and 100 mL of 60% ethanol. Transfer to a fritted-glass filter tube (30- to 60-mL capacity), and wash with six 15-mL portions of the same hydrochloric acid–60% ethanol mixture, followed by 60% ethanol until the filtrate is free of chlorides. Finally, wash with 20 mL of ethanol, dry for 2.5 h in an oven at 105°, cool, and weigh. Transfer exactly one-tenth of the total net weight of the now ash-free, dried sample (representing 0.5 g of the original unwashed sample) to a 250-mL conical flask, and moisten the sample with 2 mL of ethanol. Add 100 mL of recently boiled and cooled distilled water, stopper, and swirl occasionally until a complete solution is formed. Add 5 drops of phenolphthalein TS, titrate with 0.1 N sodium hydroxide, and record the results as the initial titer (V1). Add exactly 20 mL of 0.5 N sodium hydroxide, stopper, shake vigorously, and let stand for 15 min. Add exactly 20 mL of 0.5 N hydrochloric acid, and shake until the pink color disappears. Titrate with 0.1 N sodium hydroxide to a faint pink color that persists after vigorous shaking; record this value as the saponification titer (V2). Quantitatively transfer the contents of the conical flask into a 500-mL distillation flask fitted with a Kjeldahl trap and a watercooled condenser, the delivery tube of which extends well beneath the surface of a mixture of 150 mL of carbon dioxide-free water and 20.0 mL of 0.1 N hydrochloric acid in a receiving flask. To the distillation flask add 20 mL of a 1:10 sodium hydroxide solution, seal the connections, and then begin heating carefully to avoid excessive foaming. Continue heating until 80 to 120 mL of distillate has been collected. Add a few drops of methyl red TS to the receiving flask, titrate the excess acid with 0.1 N sodium hydroxide, and record the volume required, in mL, as SA. Perform a blank determination on 20.0 mL of 0.1 N hydrochloric acid, and record the volume required, in mL, as BA. Record the amide titer (BA – SA) as V3. Transfer exactly one-tenth of total net weight of the dried sample (representing 0.5 g of the original unwashed sample), and
FCC IV, Supplement 3
wet with about 2 mL of ethanol in a 50-mL beaker. Dissolve the Pectin in 25 mL of 0.125 M sodium hydroxide. Let the solution stand for 1 h, with agitation, at room temperature. Transfer quantitatively the saponified Pectin solution to a 50-mL volumetric flask, and dilute to volume with distilled water. Transfer 25.0 mL of the diluted Pectin solution to a distillation apparatus, and add 20 mL of Clark’s solution, which consists of 100 g of magnesium sulfate heptahydrate and 0.8 mL of sulfuric acid and distilled water to a total of 180 mL. The distillation apparatus consists of a steam generator connected to a round-bottom flask to which a condenser is attached. Both steam generator and the round-bottom flask are equipped with heating mantles. Start the distillation by heating the round-bottom flask containing the sample. Collect the first 15 mL of distillate separately in a measuring cylinder. Then start the steam supply and continue distillation until 150 mL of distillate has been collected in a 200-mL beaker. Quantitatively combine the distillates, titrate with 0.05 M sodium hydroxide to pH 8.5, and record the volume required, in mL, as SB. Perform a blank determination using 20 mL of distilled water. Record the required volume, in mL, as BB. Record acetate ester titer (SB – BB) as V4. Calculate the degree of amidation (as the percent of total carboxyl groups) by the formula 100 × [V3/(V1 + V2 + V3 – V4)]. Calculate the mg of galacturonic acid by the formula 19.41 × (V1 + V2 + V3 – V4). The mg of galacturonic acid obtained in this way is the content of one-tenth of the weight of the washed and dried sample. To calculate the percent galacturonic acid on a moistureand ash-free basis, multiply the number of mg obtained by 1000/x, in which x is the weight, in mg, of the washed and dried sample. If the pectin is known to be of the nonamidated type, only V1 and V2 need to be determined, and V3 may be regarded as zero in the formula for calculating mg of galacturonic acid. Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Alternatively, use the following procedure: (Note: Use deionized water throughout this procedure.) Diluted Standard Lead Solution (2 µg Pb/mL) Immediately before use, pipet 0.10 mL of a certified commercially available 1000 ppm (1000 µg/mL) Pb stock solution into a 50-mL volumetric flask containing 30 mL of water and 4 mL of 20% v/v hydrochloric acid and 4 mL of 0.1 M EDTA. Dilute to volume with water, and mix. Control Lead Solution (0.4 µg Pb/mL) Pipet 5.0 mL of the Diluted Standard Lead Solution into a 25-mL volumetric flask containing 10 mL of water, 2 mL of 20% v/v hydrochloric acid, and 2 mL of 0.1 M EDTA. Dilute to volume with water, and mix. Standard Lead Blank Solution Add 30 mL of water, 4 mL of 20% v/v hydrochloric acid, and 4 mL of 0.1 M EDTA into a 50mL volumetric flask. Dilute to volume with water, and mix. Sample Preparation Transfer 2.0 g of the sample into a clean 100-mL glass beaker, add 25 mL of nitric acid (70% v/v), cover with a watch glass, and heat at low to moderate heat on a hot
FCC IV, Supplement 3
plate in a fume hood for 2 h. Remove watch glass, and continue to heat until the sample is dry with no visible fumes. Add 0.5 mL of nitric acid, and heat to dryness. Cool to room temperature and add 2 mL of 20% v/v hydrochloric acid and 2 mL of 0.1 M EDTA. Transfer quantitatively to a 25-mL volumetric flask, then dilute to volume with water, and mix. Procedure Set up the inductively coupled plasma emission spectrometer according to manufacturer’s instructions, using the Pb emission line at 220.35 nm. Calibrate the instrument using the Standard Lead Blank Solution and the Diluted Standard Lead Solution. Then analyze the Sample Preparation and the Control Lead Solution. The sample passes the test if the lead concentration found in the Sample Preparation is equal to or less than that in the Control Lead Solution. Loss on Drying, Appendix IIC Dry at 105° for 2 h. Methanol, Ethanol, and Isopropanol The alcohols are converted to their nitrite esters, and their levels are determined by headspace gas chromatography. Internal Standard Solution Dissolve 50 mg of n-propanol in 1 L of water. Sample Solution Dissolve 100 mg of the sample in 10 mL of water, and as necessary, use sodium chloride as a dispersing agent. Standard Alcohol Solution Using a micropipet, transfer 50 mg each of methanol, ethanol, and isopropanol into a tared, 10mL beaker. Transfer the mixture, quantitatively, into a 1000-mL volumetric flask, dilute to volume with water, and mix. Sodium Nitrite Solution Dissolve 250 g of sodium nitrite in 1000 mL of water. Chromatographic System Use a suitable gas chromatograph equipped with a flame-ionization detector. Use a 90-cm × 4mm (id) glass column, with the first 15 cm packed with Chromopack (or equivalent) and the remainder packed with Porapak R 120- to 150-mesh (or equivalent). The operating conditions of the gas chromatograph are as follows: the injection port temperature is 250°, and the column temperature is 150° isothermal. Use nitrogen as the carrier gas with a flow rate of 80 mL/min. Procedure Weigh 200 mg of urea, and place it in a 25-mL amber-glass vial (Reacti-Flasks or equivalent). Purge with nitrogen for 5 min, add 1 mL of saturated oxalic acid solution, close with a rubber stopper, and swirl. Add 1 mL of Sample Solution and 1 mL of Internal Standard Solution, and simultaneously start a stopwatch (t = 0). Swirl the vial, and recap it with an open screw cap fitted with a silicone rubber septum. Swirl the vial until t = 30 s. At t = 45 s, inject through the septum 0.5 mL of Sodium Nitrite Solution. Swirl until t = 70 s, and at t = 150 s, withdraw through the septum 1.0 mL of the headspace using a pressure lock syringe (Precision Sampling Corporation, or equivalent). Inject the 1.0 mL into the injection port of the gas chromatograph. Repeat this procedure, but use 1 mL of the Standard Alcohol Solution instead of the Sample Solution. Calculation Quantify the total methanol, ethanol, and isopropanol present in 1 mL of the Sample Solution taken by the following formula: T = VMS (RMU/RMS) 0.791 + VES (REU/RES) 0.7893 + VIS (RIU/RIS) 0.7855, in which T is the total amount, in mg, of methanol, ethanol, and isopropanol in 1 mL of the Sample Solution; the subscripts M, E,
Monographs / Pectins / 37
and I refer to methanol, ethanol, and isopropanol, respectively; VS is the volume, in mL, of the corresponding alcohol in the Standard Alcohol Solution; RS is the ratio of the peak area of the corresponding alcohol in the Standard Alcohol Solution to that of npropanol in Internal Standard Solution; RU is the ratio of the peak area of the corresponding alcohol in the Sample Solution to that of n-propanol in the Internal Standard Solution; and 0.791, 0.7893, and 0.7855 are the densities, in g/mL, for methanol, ethanol, and isopropanol, respectively. Calculate the percent methanol, ethanol, and isopropanol present in the sample by the following formula: (1000T)/W, in which W is the sample weight, in mg. Sodium Methyl Sulfate Mobile Phase Prepare a 0.04 M potassium hydrogen phthalate solution by transferring 16.4 g of potassium hydrogen phthalate into a 2-L volumetric flask, dilute to volume with water, and mix. Filter the solution through a 0.45-µm pore-size filter (Millipore, or equivalent). Standard Preparation Transfer 10.0 mg of anhydrous sodium methyl sulfate into a 100-mL volumetric flask, dilute to volume with Mobile Phase, and mix. Assay Preparation Suspend about 1 g of the sample, accurately weighed, in 10.0 mL of 50% (v/v) ethanol solution. Stir for 30 min using a Teflon-coated stirring bar. Allow the suspension to precipitate, and filter. Evaporate a 1.0-mL aliquot to dryness using reduced pressure (10 mm Hg), and heat at 60°. Redissolve the residue in 1.0 mL of the Mobile Phase. Chromatographic System Use a high-performance liquid chromatograph equipped with a refractive index detector and a 25-cm × 4.6-mm column packed with Nucleosil 10SB (or equivalent) and maintained at 40°. Set the flow rate at 1 mL/min. System Suitability Three replicate injections of the Standard Preparation show a relative standard deviation of not more than 4.0% for the response factor of the sodium methyl sulfate peak obtained using the formula (AS/CS), in which AS is the peak area response of the Standard Preparation, and CS is the concentration, in mg/mL, of sodium methyl sulfate in the Standard Preparation. Procedure Inject 20 µL of the Standard Preparation followed by the Assay Preparation. Determine the peak area in the chromatograms for the Standard Preparation and Assay Preparation. Calculate the quantity in percent of sodium methyl sulfate in the sample by the formula (CSAU)/(ASW), in which CS is the concentration, in mg/mL, of sodium methyl sulfate in the Standard Preparation; AU and AS are the peak area responses obtained from the Assay Preparation and Standard Preparation, respectively; and W is the weight, in g, of the sample taken. Sulfur Dioxide Determine as directed in the general method, Appendix X, using the following method under Sample Introduction and Distillation: Transfer about 20 g of the sample, accurately weighed, into flask C, and add 20 mL of ethanol to moisten the sample. Add 400 mL of water, swirling vigorously to
38 / Polyglycerol Polyricinoleic Acid / Monographs
disperse the sample. Reassemble the apparatus, making sure that the tapered joints are clean and greased with stopcock grease, and proceed as directed under Sample Introduction and Distillation, beginning with “the nitrogen flow through the 3% Hydrogen Peroxide Solution….” Packaging and Storage
Store in well-closed containers.
This is a new monograph:
Polyglycerol Polyricinoleic Acid Glycerol Esters of Condensed Castor Oil Fatty Acids; Polyglycerol Esters of Interesterified Ricinoleic Acid; Polyglycerol Polyricinoleate R O R O (C C C O)n R H 2 H H2 n = 2–6; R = H or polyricinoleic acid ester
INS: 476
DESCRIPTION Polyglycerol Polyricinoleic Acid is prepared by esterification of polyglycerol with condensed castor oil fatty acids. The castor oil fatty acids are mainly composed of 80% to 90% ricinoleic acid. It is a clear, light brown, viscous liquid. It is soluble in ether, in hydrocarbons, and in halogenated hydrocarbons. It is insoluble in water and in alcohol. Functional Use in Foods
FCC IV, Supplement 3
Refractive Index Between 1.463 and 1.467. Saponification Value Between 170 and 210. TESTS Assay Sample Preparation Weigh about 0.5 g of sample and reflux with 20 mL of ethanolic 1 N potassium hydroxide solution for 2 h. Reduce the volume of ethanol by evaporation at 45° to 50° in a stream of nitrogen. Add 10 mL of water, and acidify with concentrated hydrochloric acid. Extract the fatty acids from the aqueous phase with successive 20-mL volumes of hexane. Wash the hexane extracts with 20 mL of water, and combine the wash with the aqueous phase. Adjust the aqueous polyol solution to pH 7.0 with aqueous potassium hydroxide solution with the aid of a pH meter. Evaporate to 2 to 3 mL under reduced pressure, and extract three times with 30 mL of boiling ethanol. Filter off any residue, and evaporate the ethanol under reduced pressure to yield a viscous liquid mixture of polyols. Transfer and dissolve 0.1 g of the mixture into a 10-mL capped vial containing 0.5 mL of warm pyridine previously dried over potassium hydroxide. Add 0.2 mL of hexamethyldisilazane, shake, add 2 mL of trimethylchlorosilate, and shake again. Place the vial on a warm plate at about 80° for 3 to 5 min. Check that white fumes are present, indicating an excess of reagent. Chromatographic System Use a suitable gas chromatograph equipped with a flame ionization detector (FID). Use a 1.5m × 4-mm (id) column packed with 3% OV-1 on 100- to 120mesh diatomite CQ or 100- to 120-mesh Gas Chrom Q, or equivalent. Program the oven temperature from 90° to 330° at 4° to 6°/min. The nitrogen carrier gas flow rate is 86 mL/min. Set the injection block temperature at 275° and the detector block temperature at 350°. Procedure Inject 2.0 µL of the Sample Preparation into the chromatograph. The resultant chromatogram displays the following sequence of peaks:
Emulsifier.
REQUIREMENTS Identification (Caution: Conduct these tests under a fume hood.) A. Fatty Acids Reflux 1 g of sample with 15 mL of 0.5 N ethanolic potassium hydroxide for 1 h. Add 15 mL of water, acidify with dilute hydrochloric acid TS (about 6 mL). Oily drops or a white to yellowish-white solid is produced that is soluble in 5 mL of hexane. B. Ricinoleic Acid Remove the hexane layer obtained in Identification Test A, extract again with 5 mL of hexane, and remove the hexane layer. The fatty acids thus extracted have a hydroxyl value corresponding to that of castor oil fatty acids (about 150 to 170). Assay Not less than 75% of di-, tri-, and tetraglycerols, and not more than 10% of polyglycerols equal to or higher than heptaglycerol. Acid Value Not more than 6. Hydroxyl Value Between 80 and 100. Iodine Value Between 72 and 103. Lead Not more than 1 mg/kg.
Identity Description
Elution Sequence of Peaks (and Typical Attenuation Settings)
1
Solvent
Overloaded
2
Glycerol
Single peak (2 × 103)
3
Cyclic diglycerols
Single peak (2 × 103)
4
Diglycerols
Single peak (32 × 103)
5
Cyclic triglycerols Single peak (2 × 103)
6
Triglycerols
Single peak (16 × 103)
7
Cyclic tetraglycerols
Single peak (2 × 103)
8
Tetraglycerols
Multiple peak (8 × 103)
9
Pentaglycerols
Single peak (4 × 103)
10
Hexaglycerols
Single peak (2 × 103)
11
Heptaglycerols
Single peak (2 × 103)
12
Octaglycerols
Single peak (1 × 103)
13
Nonaglycerols
Barely discernible in the tail of peak 12
FCC IV, Supplement 3
Monographs / Pork Collagen / 39
Calculation Measure each peak area, and correct for attenuation changes to obtain the corrected area (SN) of each peak. Calculate the percentage of the total di-, tri-, and tetraglycerols using the following formula:
in which SN is the corrected area of the corresponding peak.
Ash (Total) Not more than 3.0%. Fat Not more than 14.0%. Lead Not more than 1 mg/kg. Loss on Drying Not more than 5.0%. Microbial Limits Salmonella Negative in 25 g. Protein Not less than 85.0% (including collagen).
Calculate the percentage of polyols equal to or greater than heptaglycerol using the following formula:
TESTS
[(∑ S3 to S8)/(∑ S3 to S13)]100,
[(∑ S11 to S13)/(∑ S3 to S13)]100, in which SN is the corrected area of the corresponding peak. Acid Value Determine as directed for Method II under Acid Value, Appendix VII. Hydroxyl Value Determine as directed for Method II under Hydroxyl Value, Appendix VII. Iodine Value Determine as directed under Iodine Value, Appendix VII. Lead Prepare and test a 3-g sample as directed for organic compounds under the Lead Limit Test, Appendix IIIB, using 3 µg of lead ion (Pb) in the control. Refractive Index Determine as directed under Refractive Index, Appendix IIB, using an Abbé or other refractometer of equal or greater accuracy. Saponification Value Determine as directed under Saponification Value, Appendix VII, using a 4-g sample. Packaging and Storage
Store in well-closed containers.
This is a new monograph:
Pork Collagen
DESCRIPTION Pork Collagen occurs as a light tan powder. It is a mixture of proteins containing 40% to 50% collagen, a scleroprotein occurring in animal tendons, ligaments, and connective tissue. It is derived from porcine fatty trimmings gathered from the production of fresh pork meat. During processing, the raw material (pork fatty tissue) is ground, heated, and stabilized, followed by centrifugal separation to remove the fat. The partially defatted tissue is then dried and further reduced in fat content, resulting in a highprotein material that may be milled or ground into powder or granular form. It is dispersible in water, and forms thermally reversible gels. Functional Use in Foods
Binder; purge reduction.
REQUIREMENTS Identification Pork Collagen contains not less than 5.52% hydroxyproline, corresponding to 40.0% collagen, as determined by the Hydroxyproline test below. Assay Not less than 40.0% collagen.
Assay (Based on AOAC Method 990.26) Buffer Solution Transfer 30 g of citric acid monohydrate, 15 g of sodium hydroxyde, and 90 g of sodium acetate trihydrate into a 1-L volumetric flask containing 500 mL of water. Add 290 mL of 1-propanol. Adjust the pH to 6.0 with acid or base, and fill to volume with water. Oxidant Solution Weigh 1.41 g of chloramine-T, and dissolve it in 100 mL of the Buffer Solution. The solution is stable for 1 week when stored in dark bottles at 4°. Color Reagent Dissolve 10 g of 4-dimethylaminobenzaldehyde in 35 mL of 60% w/w perchloric acid. Prepare daily. Caution: Perform tests involving perchloric acid under a corrosion-resistant fume hood. Hydroxyproline Standard Solution (600 µg/mL) Weigh 60 mg of trans-4-hydroxyproline (Sigma, or equivalent) and transfer into a 100-ml volumetric flask. Dissolve and dilute to volume with water. The solution is stable for up to 2 months at 4°. Standard Curve Pipet 5 mL of the Hydroxyproline Standard Solution into a 500-mL volumetric flask, and fill to volume with water. Prepare this solution on the day of use. Pipet 10-, 20-, 30-, and 40-mL volumes into separate 100-mL volumetric flasks, and fill to volume with water. These solutions contain 0.6, 1.2, 1.8, and 2.4 µg/mL of hydroxyproline, respectively, and must be prepared on the day of use. Transfer 2.0 mL of each solution into four separate test tubes, and 2.0 mL of water into a fifth tube to use as a blank. Add 1.0 mL of Oxidant Solution to each tube, shake, and let stand for about 30 min. Add 2.0 mL of Color Reagent to each tube, mix thoroughly, cap the tubes with foil or screw caps, and place them in a water bath at 60° ± 0.5° for exactly 15 min. Cool the tubes in running water for 3 min, and dry the outside of the tubes. Measure the absorbance of each solution against the blank in 10-mm glass cells, using an appropriate spectrophotometer, at 558 nm. Draw a standard curve by plotting the absorbance values on the Y-axis and the hydroxyproline, in µg/2 mL, on the X-axis. Procedure Accurately weigh 4.0 g of sample and transfer into an Erlenmeyer flask. Add 30 mL of 7 N sulfuric acid, cover with a watch glass, and place the flasks in a drying oven at 105° for 16 h. Caution: Use an oven resistant to corrosion by acids such as those used in analysis involving perchloric acid. Use caution in handling hot hydrolysate. Transfer the hot hydrolysate quantitatively into a 500-mL volumetric flask with the aid of water. Dilute to volume with water, and mix. Filter some of the solution into a 100-mL Erlenmeyer flask. The filtrate is stable for up to 2 weeks at 4°. Dilute the filtrate with water in a volumetric flask so that the concentration
40 / Potassium Phosphate, Monobasic / Monographs
of hydroxyproline in the final dilution will be in the range of 0.5 to 2.4 µg/2 mL (dilution of 5 mL of filtrate to 100 mL is usually suitable). Record the volume of filtrate used as V. Determine as directed under Standard Curve, beginning with “Transfer 2.0 mL of each solution….” Calculation Calculate the hydroxyproline content (H), in percent, in the sample by the equation H = (X × 2.5)/(W × V), in which X is the hydroxyproline content, in µg/2 mL, obtained from the Standard Curve; W is the weight, in g, of the sample; and V is the volume, in mL, of filtrate used. Calculate the percent of collagen in the sample by multiplying the percent hydroxyproline by 7.25. Ash (Total) Determine as directed under Ash (Total), Appendix IIC. Fat Transfer 1 g of sample, accurately weighed, to a fat-extraction flask, add 10 mL of water, and shake until homogeneous (warm if necessary). Add approximately 1 mL of ammonium hydroxide, and heat in a water bath for 15 min at 60° to 70°, shaking occasionally. Add 10 mL of alcohol, and mix well. Add 25 mL of peroxide-free ether, stopper, and shake vigorously for 1 min; allow to cool if necessary; add 25 mL of petroleum ether; and shake vigorously. Allow the layers to separate and clarify or centrifuge to expedite the process. Decant the organic layer into a suitable flask or dish, and repeat the extraction twice with 15 mL each of ether and petroleum ether for each extraction. Evaporate the combined ether extractions on a steam bath, and dry the residue to a constant weight at 102°, or 70° to 75° at less than 50 mm Hg. Calculate the percent of fat in the sample taken by the formula (R × 100)/S, in which R is the weight, in mg, of the residue and S is the weight, in mg, of the sample taken. Lead Determine as directed for Method II in the Atomic Absorption Spectrophotometric Graphite Furnace Method under the Lead Limit Test, Appendix IIIB, using a 10-g sample. Loss on Drying Determine as directed under Loss on Drying, Appendix IIC. Microbial Limits Salmonella Determine as directed in chapter 5 of the FDA Bacteriological Analytical Manual, Eighth Edition, 1998. Protein Determine as directed under Nitrogen Determination, Appendix IIIC. The percent protein equals percent N × 6.25. Packaging and Storage
Store in tight containers.
FCC IV, Supplement 3
Revision: Fluoride test corrected; Heavy Metals (as Pb) specification and determination deleted. Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limit for this substance: Cadmium, not more than 2 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
Potassium Phosphate, Monobasic Potassium Biphosphate; Potassium Dihydrogen Phosphate; Monopotassium Phosphate KH2PO4 INS: 340(i)
Formula wt 136.09 CAS: [7778-77-0]
DESCRIPTION Colorless crystals or a white granular or crystalline powder. It is odorless, and is stable in air. It is freely soluble in water, but is insoluble in alcohol. The pH of a 1:100 solution is between 4.2 and 4.7. Functional Use in Foods etary supplement.
Buffer; sequestrant; yeast food; di-
REQUIREMENTS Identification A 1:20 solution gives positive tests for Potassium and for Phosphate, Appendix IIIA. Assay Not less than 98.0% of KH2PO4 after drying. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 10 mg/kg. Insoluble Substances Not more than 0.2%. Lead Not more than 2 mg/kg. Loss on Drying Not more than 1%. TESTS Assay Transfer about 5 g of the sample, previously dried at 105° for 4 h and accurately weighed, into a 250-mL beaker, add 100 mL of water and 5.0 mL of 1 N hydrochloric acid, and stir until the sample is completely dissolved. Place the electrodes of a suitable pH meter in the solution, and slowly titrate the excess acid, stirring constantly, with 1 N sodium hydroxide to the inflection point occurring at about pH 4. Record the buret reading, and calculate the volume (A), if any, of 1 N hydrochloric acid consumed by the sample. Continue the titration with 1 N sodium hydroxide until the inflection point occurring at about pH 8.8 is reached, record the buret reading, and calculate the volume (B) of 1 N sodium hydroxide required in the titration between the two inflection points (pH 4 and pH 8.8). Each mL of the volume B – A of 1 N sodium hydroxide is equivalent to 136.1 mg of KH2PO4. Arsenic A solution of 1 g in 10 mL of water meets the requirements of the Arsenic Test, Appendix IIIB.
FCC IV, Supplement 3
Monographs / Potassium Pyrophosphate / 41
Fluoride Determine on a 2-g sample as directed in Method IV under the Fluoride Limit Test, Appendix IIIB. Insoluble Substances Dissolve 10 g in 100 mL of hot water, and filter through a tared filtering crucible. Wash the insoluble residue with hot water, dry at 105° for 2 h, cool, and weigh. Lead A 10-g sample meets the requirements of the APDC Extraction Method for Lead, Appendix IIIB. Loss on Drying, Appendix IIC Dry at 105° for 4 h. Packaging and Storage
Store in tight containers.
Revision: Fluoride test corrected; Heavy Metals (as Pb) specification and determination deleted. Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limit for this substance: Cadmium, not more than 2 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
Potassium Phosphate, Tribasic Tripotassium Phosphate K3PO4
Formula wt 212.27
INS: 340(iii)
Packaging and Storage
Store in tight containers.
CAS: [7778-53-2]
Revision: Fluoride test corrected; Heavy Metals (as Pb) specification and determination deleted.
DESCRIPTION Tribasic Potassium Phosphate is anhydrous or may contain one molecule of water of hydration. It occurs as white, odorless, hygroscopic crystals or granules. It is freely soluble in water, but is insoluble in alcohol. The pH of a 1:100 solution is about 11.5. Functional Use in Foods
Pass a stream of carbon dioxide-free air, in fine bubbles, through the solution for 30 min to expel carbon dioxide, covering the beaker loosely to prevent any loss by spraying. Wash the cover and sides of the beaker with a few mL of water, and place the electrodes of a suitable pH meter in the solution. Titrate the solution with 1 N sodium hydroxide to the inflection point occurring at about pH 4, then calculate the volume (A) of 1 N hydrochloric acid consumed. Protect the solution from absorbing carbon dioxide, and continue the titration with 1 N sodium hydroxide until the inflection point occurring at about pH 8.8 is reached. Calculate the volume (B) of 1 N sodium hydroxide consumed in this titration. When A is equal to or greater than 2B, each mL of the volume B of 1 N sodium hydroxide is equivalent to 212.3 mg of K3PO4. When A is less than 2B, each mL of the volume A – B of 1 N sodium hydroxide is equivalent to 212.3 mg of K3PO4. Arsenic A solution of 1 g in 10 mL of water meets the requirements of the Arsenic Test, Appendix IIIB. Fluoride Determine on a 2-g sample as directed in Method IV under the Fluoride Limit Test, Appendix IIIB. Insoluble Substances Dissolve 10 g in 100 mL of hot water, and filter through a tared filtering crucible. Wash the insoluble residue with hot water, dry at 105° for 2 h, cool, and weigh. Lead A 10-g sample meets the requirements of the APDC Extraction Method for Lead, Appendix IIIB. Loss on Ignition, Appendix IIC Ignite at about 800° for 30 min.
Emulsifier.
Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limit for this substance: Cadmium, not more than 2 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
REQUIREMENTS
Potassium Pyrophosphate
Identification A 1:20 solution gives positive tests for Potassium and for Phosphate, Appendix IIIA. Assay Not less than 97.0% of K3PO4, calculated on the ignited basis. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 10 mg/kg. Insoluble Substances Not more than 0.2%. Lead Not more than 2 mg/kg. Loss on Ignition K3PO4 (anhydrous): not more than 3.0%; K3PO4.H2O (monohydrate): between 8.0% and 20.0%.
Tetrapotassium Pyrophosphate
TESTS Assay Dissolve an accurately weighed quantity of the sample, equivalent to about 8 g of anhydrous K3PO4, in 40 mL of water in a 400-mL beaker, and add 100.0 mL of 1 N hydrochloric acid.
K4P2O7 INS: 452(ii)
Formula wt 330.34 CAS: [7320-34-5]
DESCRIPTION Colorless crystals, or a white, granular solid. It is hygroscopic. It is very soluble in water, but is insoluble in alcohol. The pH of a 1:100 solution is about 10.5. Functional Use in Foods
Emulsifier; texturizer.
42 / Potassium Sorbate / Monographs
REQUIREMENTS Identification A. A 1:20 solution gives positive tests for Potassium, Appendix IIIA. B. Dissolve 100 mg of the sample in 100 mL of 1.7 N nitric acid. Add 0.5 mL of this solution to 30 mL of quimociac TS. A yellow precipitate does not form. Heat the remaining portion of the sample solution for 10 min at 95°, and then add 0.5 mL of the solution to 30 mL of quimociac TS. A yellow precipitate forms immediately. Assay Not less than 95.0% of K4P2O7, calculated on the ignited basis. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 10 mg/kg. Insoluble Substances Not more than 0.1%. Lead Not more than 2 mg/kg. Loss on Ignition Not more than 0.5%. TESTS
Revision: Color of sample in Description corrected; Heavy Metals (as Pb) specification and determination deleted.
Potassium Sorbate 2,4-Hexadienoic Acid, Potassium Salt CH3CH CHCH
CHCOOK
C6H7KO2
Formula wt 150.22
INS: 202
CAS: [590-00-1]
DESCRIPTION White to off-white crystals, crystalline powder, or pellets. It decomposes at about 270°. Functional Use in Foods
Preservative.
REQUIREMENTS
Assay Dissolve about 600 mg, accurately weighed, in 100 mL of water in a 400-mL beaker, and using a pH meter, adjust the pH of the solution to exactly 3.8 with hydrochloric acid. Add 50 mL of a 1:8 solution of zinc sulfate (125 g of ZnSO4.7H2O dissolved in water, diluted to 1000 mL, filtered, and adjusted to pH 3.8), and allow to stand for 2 min. Titrate the liberated acid with 0.1 N sodium hydroxide until a pH of 3.8 is again reached. After each addition of sodium hydroxide near the endpoint, time should be allowed for any precipitated zinc hydroxide to redissolve. Each mL of 0.1 N sodium hydroxide is equivalent to 16.52 mg of K4P2O7. Arsenic A solution of 1 g in 35 mL of water meets the requirements of the Arsenic Test, Appendix IIIB. Fluoride Determine on a 2-g sample as directed in Method IV under the Fluoride Limit Test, Appendix IIIB. Insoluble Substances Dissolve 10 g in 100 mL of hot water, and filter through a tared filtering crucible. Wash the insoluble residue with hot water, dry at 105° for 2 h, cool, and weigh. Lead A 10-g sample meets the requirements of the APDC Extraction Method for Lead, Appendix IIIB. Loss on Ignition Ignite at about 800° for 30 min. Packaging and Storage
FCC IV, Supplement 3
Store in tight containers.
Identification A. A 1:10 solution responds to the flame test for Potassium, Appendix IIIA. B. To 2 mL of a 1:10 solution, add a few drops of bromine TS. The color is discharged. Assay Not less than 98.0% and not more than 101.0% of C6H7KO2, calculated on the dried basis. Acidity (as sorbic acid) Passes test (about 1%). Alkalinity (as K2CO3) Passes test (about 1%). Loss on Drying Not more than 1.0%. TESTS Assay Dissolve about 250 mg, accurately weighed, in 40 mL of glacial acetic acid in a 250-mL, glass-stoppered Erlenmeyer flask, warming if necessary to effect solution. Cool to room temperature, add 2 drops of crystal violet TS, and titrate with 0.1 N perchloric acid in glacial acetic acid to a blue-green endpoint that persists for at least 30 s. Perform a blank determination (see General Provisions), and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 15.02 mg of C6H7KO2. Acidity or Alkalinity Dissolve 1.1 g in 20 mL of water and add 3 drops of phenolphthalein TS. If the solution is colorless, titrate with 0.1 N sodium hydroxide to a pink color that persists for 15 s. Not more than 1.1 mL is required. If the solution is pink in color, titrate with 0.1 N hydrochloric acid. Not more than 0.8 mL is required to discharge the pink color. Loss on Drying, Appendix IIC Dry at 105° for 3 h. Packaging and Storage
Store in tight containers.
FCC IV, Supplement 3
Monographs / L-Proline / 43
Revision: Fluoride test corrected; Heavy Metals (as Pb) specification and determination deleted. Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limit for this substance: Cadmium, not more than 2 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
Loss on Drying, Appendix IIC Dry at about 105° for 1 h. Packaging and Storage
Store in tight containers.
Revision: Identification test corrected; Heavy Metals (as Pb) specification and determination deleted. L-Proline
Potassium Tripolyphosphate Pentapotassium Triphosphate; Potassium Triphosphate K5P3O10
Formula wt 448.41
INS: 450(v)
CAS: [13845-36-8]
L-2-Pyrrolidinecarboxylic Acid
COOH N H
C5H9NO2
H
Formula wt 115.13 CAS: [147-85-3]
DESCRIPTION White granules or a white powder. It is hygroscopic and is very soluble in water. The pH of a 1:100 solution is between 9.2 and 10.1. Functional Use in Foods
Texturizer.
DESCRIPTION White crystals or a crystalline powder. It is very soluble in water and in alcohol, but is insoluble in ether. Functional Use in Foods
Nutrient; dietary supplement.
REQUIREMENTS Identification A. A 1:20 solution gives positive tests for Potassium, Appendix IIIA. B. Add a few drops of silver nitrate TS to 1 mL of a 1:100 solution. A white precipitate is formed that is soluble in 1.7 N nitric acid. Assay Not less than 85.0% of K5P3O10. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 10 mg/kg. Insoluble Substances Not more than 2.0%. Lead Not more than 2 mg/kg. Loss on Drying Not more than 0.7%.
REQUIREMENTS Identification Heat 5 mL of a 1:1000 solution of the sample with 1 mL of triketohydrindene hydrate TS (ninhydrin TS). A yellow color is produced. Assay Not less than 98.5% and not more than 101.5% of C5H9NO2 after drying. Lead Not more than 10 mg/kg. Loss on Drying Not more than 0.3%. Residue on Ignition Not more than 0.1%. Specific Rotation [α]20° D : Between –84.0° and –86.3° after drying. TESTS
TESTS Assay Proceed as directed in the Assay in the monograph for Sodium Tripolyphosphate. Calculate the quantity, in mg, of K5P3O10 in the sample taken by the formula 0.650 × 25V. Arsenic A solution of 1 g in 35 mL of water meets the requirements of the Arsenic Test, Appendix IIIB. Fluoride Determine on a 2-g sample as directed in Method IV under the Fluoride Limit Test, Appendix IIIB. Insoluble Substances Dissolve 10 g in 100 mL of hot water, and filter through a tared filtering crucible. Wash the insoluble residue with hot water, dry at 105° for 2 h, cool, and weigh. Lead A 10-g sample meets the requirements of the APDC Extraction Method for Lead, Appendix IIIB.
Assay Dissolve about 220 mg of the sample, previously dried at 105° for 3 h and accurately weighed, in 3 mL of formic acid and 50 mL of glacial acetic acid, add 2 drops of crystal violet TS, and titrate with 0.1 N perchloric acid to a bluish green endpoint. Perform a blank determination (see General Provisions), and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 11.51 mg of C5H9NO2. Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Loss on Drying, Appendix IIC Dry at 105° for 3 h. Residue on Ignition, Appendix IIC Ignite 1 g as directed in the general method.
44 / Quinine Hydrochloride / Monographs
FCC IV, Supplement 3
Specific Rotation, Appendix IIB Determine in a solution containing 4 g of a previously dried sample in sufficient water to make 100 mL. Packaging and Storage containers.
Store in well-closed, light-resistant
Revision: Barium and Heavy Metals (as Pb) specifications and determinations deleted.
Quinine Hydrochloride HO H
N
H3CO
H
H CH2
.HCl.2H2O
N
C20H24N2O2.HCl.2H2O
Formula wt 396.91 CAS: [130-89-2]
DESCRIPTION White, silky, glistening needles. It is odorless, has a very bitter taste, and effloresces when exposed to warm air. Its solutions are neutral or alkaline to litmus. One g dissolves in 16 mL of water, in 1 mL of alcohol, in about 7 mL of glycerin, and in about 1 mL of chloroform. It is very slightly soluble in ether. Functional Use in Foods
Flavoring agent.
REQUIREMENTS Identification A. To 5 mL of a 1:1000 solution of the sample add 1 or 2 drops of bromine TS followed by 1 mL of 6 N ammonium hydroxide. The liquid acquires an emerald green color due to the formation of thalleioquin. B. A 1:100 solution is levorotatory (see Appendix IIB). C. It gives positive tests for Chloride, Appendix IIIA. Assay Not less than 99.0% and not more than 101.5% of C20H24N2O2.HCl, calculated on the dried basis. Chloroform–Alcohol Insoluble Substances Passes test. Loss on Drying Not more than 10.0%. Other Cinchona Alkaloids Passes test. Readily Carbonizable Substances Passes test. Residue on Ignition Not more than 0.15%. Specific Rotation [α]25° D : Between –247° and –252°. Sulfate Not more than 0.05%. TESTS Assay Dissolve about 150 mg of the sample, accurately weighed, in 20 mL of acetic anhydride, add 2 drops of malachite
green TS and 5.5 mL of mercuric acetate TS, and titrate with 0.1 N perchloric acid from a microburet to a yellow endpoint. Perform a blank determination (see General Provisions). Each mL of 0.1 N perchloric acid is equivalent to 17.99 mg of C20H24N2O2.HCl. Chloroform–Alcohol Insoluble Substances One g dissolves completely in 7 mL of a mixture of 2 volumes of chloroform and 1 volume of absolute alcohol. Loss on Drying, Appendix IIC Dry at 120° for 3 h. Other Cinchona Alkaloids Dissolve about 2.5 g in 60 mL of water in a separator, add 10 mL of 6 N ammonium hydroxide, extract the mixture successively with 30 mL and 20 mL of chloroform, and evaporate the combined chloroform extracts to dryness on a steam bath. Dissolve 1.5 g of the residue in 25 mL of alcohol, dilute the solution with 50 mL of hot water, add 1 N sulfuric acid (about 5 mL) until the solution is acid, using 2 drops of methyl red TS as the indicator, and neutralize the excess of acid with 1 N sodium hydroxide. Evaporate the solution to dryness on a steam bath, powder the residue, and agitate it in a test tube with 20 mL of water at 65° for 30 min. Cool the mixture to 15°, macerate it at this temperature for 2 h with occasional shaking, and then filter it through a filter paper (8 to 10 cm). Transfer 5 mL of the filtrate, at a temperature of 15°, to a test tube, and mix it gently, with shaking, with 6 mL of 6 N ammonium hydroxide (which must contain between 10% and 10.2% of NH3, have a temperature of 15°, and be added at once). A clear liquid is produced. Readily Carbonizable Substances, Appendix IIB Dissolve 100 mg in 2 mL of 95% sulfuric acid. The solution is no darker than Matching Fluid M. Residue on Ignition Ignite 1 g as directed in the general method, Appendix IIC. Specific Rotation, Appendix IIB Determine in a solution containing 200 mg in 10 mL of 0.1 N hydrochloric acid. Sulfate, Appendix IIIB Any turbidity produced by a 500-mg sample does not exceed that shown in a control containing 250 µg of sulfate (SO4). Packaging and Storage tainers.
Store in tight, light-resistant con-
Revision: Description and Functional Use in Foods modified, Heavy Metals (as Pb) specification and determination deleted.
Rapeseed Oil, Fully Hydrogenated Fully Hydrogenated Rapeseed Oil INS: 441
CAS: [84681-71-0]
DESCRIPTION Fully Hydrogenated Rapeseed Oil occurs as a white, waxy, odorless solid that is a mixture of triglycerides. The saturated fatty acids are found in the same proportions that result from the full hydrogenation of fatty acids occurring in natural high erucic acid rapeseed oil. The rapeseed oil is obtained from Brassica juncea,
FCC IV, Supplement 3
Monographs / Rapeseed Oil, Superglycerinated / 45
Brassica napus, and Brassica rapa of the family Cruciferae. It is made by hydrogenating high erucic acid rapeseed oil in the presence of a nickel catalyst at temperatures not exceeding 245°. Functional Use in Foods Cooking or salad oil; component of margarine or shortening; coating agent; emulsifying agent; stabilizer; thickener; formulation aid; texturizer. REQUIREMENTS Labeling Rapeseed oil products that have been fully hydrogenated should be labeled as Fully Hydrogenated Rapeseed Oil. Label to indicate 1-Monoglyceride content. Identification Fully Hydrogenated Rapeseed Oil exhibits the following composition profile of fatty acids as determined under Fatty Acid Composition, Appendix VII.
1-Monoglyceride Content Determine as directed in the general method, Appendix VII. Peroxide Value Proceed as directed under Peroxide Value in the monograph for Hydroxylated Lecithin. However, after the addition of saturated potassium iodide and mixing, mix the solution for only 1 min and begin the titration immediately instead of allowing the solution to stand for 10 min. Residue on Ignition Ignite 5 g as directed in the general method, Appendix IIC. Unsaponifiable Matter Proceed as directed under Unsaponifiable Matter, Appendix VII. Water Proceed as directed under Water Determination using the Karl Fischer Titrimetric Method, Appendix IIB. However, in place of 35 to 40 mL of methanol, use 50 mL of a 1:1 chloroform:methanol mixture to dissolve the sample. Packaging and Storage
Fatty Acid:
14:0
16:0
18:0
18:1
18:2
Weight % (Range):
<1.0
3–5
38–42 <1.0
<1.0
Fatty Acid:
20:0
20:1
22:0
24:0
Weight % (Range):
8–10
<1.0
42–50 <1.0
22:1
1.0–2.0
Acid Value Not more than 6. Color (AOCS-Wesson) Not more than 1.5 red/15 yellow. Erucic Acid Not more than 1.0%. Free Fatty Acids (as oleic acid) Not more than 2.0%. Iodine Value Not more than 4. Lead Not more than 0.1 mg/kg. Peroxide Value Not more than 2.0 meq/kg. Residue on Ignition Not more than 0.5%. Unsaponifiable Matter Not more than 1.5%. Water Not more than 0.05%. ADDITIONAL REQUIREMENTS The following specification should conform to the representations of the vendor: 1-Monoglyceride Content. TESTS Acid Value Determine as directed for Acid Value, Method II, under Fats and Related Substances, Appendix VII. Color Proceed as directed for Color (AOCS-Wesson) under Fats and Related Substances, Appendix VII. Use a 13.34-cm cell. Erucic Acid Determine as part of Fatty Acid Composition, Appendix VII. Free Fatty Acids Proceed as directed under Free Fatty Acids, Appendix VII, using the following equivalence factor (e) in the formula given in the procedure: Free fatty acids as oleic acid, e = 28.2. Iodine Value Proceed as directed under Modified Wijs Method, Appendix VII. Lead Determine as directed under Method II in the Atomic Absorption Spectrophotometric Graphite Furnace Method under the Lead Limit Test, Appendix IIIB, using a 1-g sample.
Store in well-closed containers.
Revision: Description and Functional Use in Foods modified, Heavy Metals (as Pb) specification and determination deleted.
Rapeseed Oil, Superglycerinated Superglycerinated Fully Hydrogenated Rapeseed Oil
DESCRIPTION Superglycerinated Rapeseed Oil occurs as a white solid. It is a mixture of mono-, di-, and triglycerides, with triglycerides as a minor component. The saturated fatty acids are found in the same proportions that result from the full hydrogenation of fatty acids occurring in natural high erucic acid rapeseed oil. The rapeseed oil is typically obtained by n-hexane extraction from Brassica juncea, Brassica napus, and Brassica rapa of the family Cruciferae. It is made by adding excess glycerin to fully hydrogenated rapeseed oil and heating, in the presence of sodium hydroxide catalyst, to about 165° under partial vacuum and steam sparging agitation. Functional Use in Foods Cooking or salad oil; component of margarine or shortening; coating agent; emulsifying agent; formulation aid; texturizer. REQUIREMENTS Labeling Indicate Rapeseed Oil products that have added glycerin (glycerol) and are fully hydrogenated as fully hydrogenated and superglycerinated Rapeseed Oil. The 1-Monoglyceride Content and Hydroxyl Value should conform to the representations of the vendor, and this should be indicated as well. Identification Superglycerinated Rapeseed Oil exhibits the same fatty acid composition as fully hydrogenated rapeseed oil. It exhibits the following composition profile of fatty acids as determined under Fatty Acid Composition, Appendix VII.
46 / Salatrim / Monographs
FCC IV, Supplement 3
Fatty Acid:
14:0
16:0
18:0
18:1
18:2
Weight % (Range):
<1.0
3–5
38–42 <1.0
<1.0
Fatty Acid:
20:0
20:1
22:0
24:0
Salatrim
Weight % (Range):
8–10
<1.0
42–50 <1.0
1.0–2.0
Short- and Long-Chain Acyl Triglyceride Molecules
22:1
This is a new monograph:
O
Acid Value Not more than 6. Color (AOCS-Wesson) Not more than 1.5 red/15 yellow. Erucic Acid Not more than 1.0%. Free Fatty Acids (as oleic acid) Not more than 2.0%. Free Glycerin Not more than 1%. Iodine Value Not more than 4. Lead Not more than 0.1 mg/kg. Peroxide Value Not more than 2.0 meq/kg. Residue on Ignition Not more than 0.5%. Unsaponifiable Matter Not more than 1.5%. Water Not more than 0.05%.
CH2OC(CH2)xCH3 O CH2OC(CH2)yCH3 O CH2OC(CH2)zCH3 in which (x + y + z) is between 14 and 42
DESCRIPTION TESTS 1-Monoglyceride Content Determine as directed in the general method, Appendix VII. Acid Value Determine as directed for Acid Value, Method II, under Fats and Related Substances, Appendix VII. Color Proceed as directed for Color (AOCS-Wesson) under Fats and Related Substances, Appendix VII. Use a 13.34-cm cell. Erucic Acid Determine as part of Fatty Acid Composition, Appendix VII. Free Fatty Acids Proceed as directed under Free Fatty Acids, Appendix VII, using the following equivalence factor (e) in the formula given in the procedure: Free fatty acids as oleic acid, e = 28.2. Free Glycerin Determine as directed in the general method, Appendix VII. Hydroxyl Value Determine as directed under Method II in the general method, Appendix VII. Iodine Value Proceed as directed under the Modified Wijs Method, Appendix VII. Lead Determine as directed under Method II in the Atomic Absorption Spectrophotometric Graphite Furnace Method under the Lead Limit Test, Appendix IIIB, using a 1-g sample. Peroxide Value Proceed as directed in Peroxide Value in the monograph for Hydroxylated Lecithin. However, after the addition of saturated potassium iodide and mixing, mix the solution for only 1 min and begin the titration immediately instead of allowing the solution to stand for 10 min. Residue on Ignition Ignite 5 g as directed in the general method, Appendix IIC. Total Monoglycerides Determine as directed in the general method, Appendix VII. Unsaponifiable Matter Proceed as directed under Unsaponifiable Matter, Appendix VII. Water Proceed as directed under Water Determination using the Karl Fischer Titrimetric Method, Appendix IIB. However, in place of 35 to 40 mL of methanol, use 50 mL of a 1:1 chloroform:methanol mixture to dissolve the sample. Packaging and Storage
Store in well-closed containers.
Salatrim ranges from a slightly viscous, clear amber liquid to a light-colored, waxy solid. Salatrim is the abbreviated name for short- and long-chain acyl triglyceride molecules. It is prepared by interesterification of triacetin, tripropionin, tributyrin, or their mixtures with hydrogenated canola, soybean, sunflower, or cottonseed oil. The process removes triglycerides with three shortchain fatty acids. Salatrim triglycerides typically contain 30 to 67 mol-% short-chain fatty acids (SCFA) and 33 to 70 mol-% longchain fatty acids (LCFA); stearic acid is the predominant LCFA. It is free of particulate matter. It is soluble in hexane, in cyclohexane, in acetone, in ether, in tetrahydrofuran, and in liquid triglyceride oils but is insoluble in water. It melts at 16° to 71° depending on triglyceride composition. Functional Use in Foods conventional fats and oils.
Reduced-energy-fat replacement for
REQUIREMENTS Identification An infrared absorption spectrum of the sample contained in a sodium chloride cell or between salt plates exhibits maxima at the same wavelengths as the typical spectrum, as shown in the section on Infrared Spectra. Assay Not less than 87% triglycerides, not less than 90% of the triglycerides with an SCFA-to-LCFA mole ratio in the range of 0.5 to 2.0, and not more than 70% by weight of saturated longchain fatty acids. Free Fatty Acids (as oleic acid) Not more than 0.5%. Lead Not more that 0.1 mg/kg. Monoglycerides Not more than 2%. Peroxide Value Not more than 2.0. Residue on Ignition Not more than 0.1%. Unsaponifiable Matter Not more than 1.0%. Water Not more than 0.3%. TESTS Assay (Excerpted with permission from J. Agric. Food Chem. 1994, 42: 453–460. Copyright 1994 American Chemical Society).
FCC IV, Supplement 3
Monoglyceride and Triglyceride Content This method permits the quantitation of Monoglycerides (MG) with one longchain fatty acid (LCFA) and Triglycerides (TG) with the same acyl carbon number (ACN) in Salatrim by high-temperature capillary gas chromatography. The ACN is the sum of the number of carbons of each carboxylic acid side-chain of each TG. For example, the ACN for tristearin is 54 (i.e., 3 × 18), and the ACNs for both dipropionylstearoylglycerol and diacetylarachidoylglycerol are 24, that is, [(2 × 3) + 18] and [(2 × 2) + 20], respectively. MG and TG are identified by comparison with standards. The weight percent of each MG and TG in Salatrim is determined from the peak areas and calibration curves constructed using data from analyses of standard solutions. MG Standards (2) Obtain monopentadecanoin (monoC15) and monostearin (mono-C18) with a minimum purity of 99% (available from Nu Check Prep., Inc., Elysian, MN). TG Standards (13) Obtain tricaproin (tri-C6), triheptanoin (tri-C7), tricaprylin (tri-C8), trinonanoin (tri-C9), tricaprin (triC10), triundecanoin (tri-C11), trilaurin (tri-C12), tritridecanoin (tri-C13), trimyristin (tri-C14), tripentadecanoin (tri-C15), tripalmitin (tri-C16), triheptadecanoin (tri-C17), and tristearin (triC18) with a minimum purity of 99% (available from Nu Check Prep., Inc., Elysian, MN). Internal Standard Stock Solution Dissolve 200 mg of triC11 in 2 L of spectroscopic-grade undecane/toluene (95/5 v/v). Standard Solutions (Group 1) Add the two MG Standards to each of 7 10-mL volumetric flasks so that each flask, respectively, contains 500, 250, 125, 62.5, 31, 15.6, and 7.8 mg/L of each MG Standard when filled to volume with Internal Standard Stock Solution. Standard Solutions (Group 2) Add the 13 TG Standards to each of 22 10-mL volumetric flasks, so that each flask, respectively, contains 1600, 800, 400, 200, 100, 50, 32, 25, 20, 18, 16, 14, 12, 10, 9, 8, 7, 6, 5, 4, 3, and 2 mg/L of each TG Standard when filled to volume with Internal Standard Stock Solution. Salatrim Solution Accurately weigh 2 g of Salatrim into a 1-L volumetric flask. Dilute to volume with Internal Standard Stock Solution. Procedure Equipment A Hewlett-Packard 5890 Series II GC equipped with a flame-ionization detector (FID), a pressureprogrammable on-column injector, an HP 7673 auto-sampler, and an HP Series II integrator, or the equivalent. A Chrompack SIMDIST CB fused-silica GC column (Chrompack Inc., Raritan, NJ) with a 5-m × 0.32-mm id and a 0.1-µm film thickness, or the equivalent. A deactivated fused-silica precolumn (0.5-m × 0.53mm id) coupled to the analytical column via a butt connector (Quadrex Corp., New Haven, CT), or the equivalent. Set the oven temperature to ramp 140° to 350° at a rate of 10°/min (total run time of 21.0 min). Set the track mode to “on” (injector temperature follows the oven temperature conditions). Set the injection mode to on-column injection. Set the FID at 375°. Set the hydrogen carrier gas constant flow mode to “on” with a pressure of 5.5 psi (140°). Quantitation of MG Determine the calibration curve and response factor (RF) for Mono-C15 and Mono-C18 by the following procedure: Analyze each of the Standard Solutions (Group 1) using a sample injection volume of 0.5 µL. From each chro-
Monographs / Salatrim / 47
matogram, establish the response factors (RFi) for the two MG Standards using the following formula: RFi = (CIS/Ci) × (Ai/AIS), in which CIS is the concentration, in mg/L, of the Internal Standard Stock Solution; Ci is the concentration, in mg/L, of an MG; Ai is the peak area of an MG; and AIS is the peak area of the Internal Standard Stock Solution. For each MG, construct a calibration curve by plotting the peak area ratios of (Ai/AIS) (x-axis) versus the RFi (y-axis) for each solution. Weight Percent of MG Analyze the Salatrim sample using a sample injection of 0.5 µL. From the chromatograms, obtain the peak area of each MG (Ai) and of the Internal Standard Stock Solution (AIS). Calculate the peak area ratio (Ai/AIS) and determine the RF for each MG (RFi) from the calibration curve. The concentration, in µg/mL, of each MG (Ci) in the sample is Ci = (CIS/RFi) × (Ai/AIS), in which CIS is the concentration of the Internal Standard Stock Solution. The weight percent [(W%)i] of each MG in the sample is (W%)i = (Ci/CT) × 100, in which CT is the concentration, in mg/L, of the Salatrim Solution. The total weight percent of MG in the sample is ∑i (W%)i. Quantitation of TG with the Same ACN To determine the RF for TG Standards, analyze each of the Standard Solutions (Group 2) using a sample injection volume of 0.5 µL. Determine the RF for each TG Standard (j) by the formula RFnj = (CIS/Cnj) × (Anj/AIS), in which CIS is the concentration, in mg/L, of the Internal Standard Solution; Cnj is the concentration, in mg/L, of each TG Standard; Anj is the peak area of each TG Standard with an acetyl carbon number equaling n (n = 18–54 and the acetyl carbon number of the TG Standard is as follows: tri-C6, 18; tri-C7, 21; tri-C8, 24; tri-C9, 27; tri-C10, 30; tri-C11, 33; tri-C12, 36; triC13, 39; tri-C14, 42; tri-C15, 45; tri-C16, 48; tri-C17, 51; and triC18, 54); and AIS is the peak area of the Internal Standard Stock Solution. The relative peak area of each TG Standard with ACN = n and concentration Cnj to that of the Internal Standard Solution is given by RAnj = Anj/AIS. Note: The notations “j + 1,” “j,” and “j – 1” denote consecutive concentration values in the series of standard solutions. For example, for a TG Standard with ACN = n and concentrations of 100, 200, and 400 mg/L, the relative peak areas RAnj+1 and RAnj–1 correspond to data for standards with concentrations of 400 mg/L and 100 mg/L, respectively. The RF and relative peak areas for each TG with ACN = n + 1 and with ACN = n + 2 are calculated from the measured RF and RA values for TG standards with ACN = n and n + 3 at the same concentration, Cnj, according to the following:
48 / Salatrim / Monographs
RFn + 1j = RFnj + (RFn + 3j – RFnj) × 1⁄3 RAn + 1j = RAnj + (RAn + 3j – RAnj) × 1⁄3 RFn + 2j = RFnj + (RFn + 3j – RFnj) × 2⁄3 RAn + 2j = RAnj + (RAn + 3j – RAnj) × 2⁄3 For the Salatrim sample, calculate the RF for the TG with a relative peak area RAnj by the formula RFnj = RFnj – 1 + (RFnj + 1 – RFnj –1) × [(RAnj – RAnj – 1)/(RAnj + 1 – RAnj –1)], in which RFnj – 1 and RFnj + 1 are the response factors, and RAnj – 1 and RAnj + 1 are the relative peak areas, respectively, of the TG Standard with the same ACN value. RAnj + 1 and RAnj – 1 must meet the following condition: RAnj – 1 ≤ RAnj < RAnj + 1, in which RAnj is the ratio of the peak area of the TG in Salatrim with ACN = n, (Anj), to the peak area for the Internal Standard Solution (AIS). To determine the weight percent of Salatrim TG components, the concentration (mg/L) of TG in the Salatrim sample with ACN = n is given by Cnj = (CIS/RFnj) × (Anj/AIS), in which CIS is the concentration, in mg/L, of the Internal Standard Stock Solution. The weight percent of TG with ACN = n in Salatrim is (W%)n = (Cnj/CT) × 100, in which CT is the concentration, in mg/L, of the Salatrim Solution. The total weight percent of TG in the sample is ∑n (W%)n. Short-Chain Fatty Acids (SCFA)/Long-Chain Fatty Acids (LCFA) Mole Ratio Apparatus Gas chromatograph with flame ionization detector (Hewlett-Packard 5890 Series II, or the equivalent) equipped with a 5-µL syringe for 0.32-mm (id) columns. Automatic sampler (HP 7673, or equivalent). Chromatographic data system or integrator (HP 3365 Series II software, or the equivalent). Retention gap, deactivated fused silica, 1-mm × 0.32mm (id) with capillary column connectors. DB 5-HT, 15-m × 0.32-mm (id) fused silica capillary column (J&W Scientific, Inc., 91 Blue Ravine Road, Folsom, CA 95630-4714, catalog number 123-5711, or the equivalent). Crimp caps and vials (HP 51813375, or the equivalent) for an on-line autosampler. 0.5 N Sodium Butoxide Transfer 9.62 g of sodium butoxide solution (50% in butanol) into a 100-mL volumetric flask, dilute to volume with 1-butanol, and mix. Butyl Ester Standards Butyl butyrate (98%); n-butyl acetate (99%); butyl propionate; butyl palmitate; butyl stearate (93%). Standard Reference Solution (Note: Melt the butyl stearate standard before sampling.) Accurately weigh about 50 mg of each butyl ester standard, and transfer them into a single 100-mL volumetric flask. Dilute to volume with HPLC-grade hexane
FCC IV, Supplement 3
(95%), and mix. More than one Standard Reference Solution may be necessary if impurities co-elute with standard peaks. Sample Solution Accurately weigh approximately 50 mg of melted Salatrim, and transfer it into a 100-mL volumetric flask. Dilute to volume with hexane, and mix. Procedure For each sample (hexane blank, Standard Reference Solution, and Sample Solution) to be assayed, pipet 5.0 mL of solution into a clean 8-mL clear glass vial. Add 0.5 mL of 0.5 N sodium butoxide, seal, and shake vigorously. The solution will turn yellow. For the hexane blank and the Sample Solutions only, allow the solution to stand for 2 min. Neutralize the mixture by adding 1.0 mL of 0.5 N hydrochloric acid. Seal the vial, and shake well until the solution is clear. Check the pH with pH paper: The solution should be acidic. If it is not, the column will degrade. Note: 1-butanol and water may be substituted for 0.5 N sodium butoxide and 0.5 N hydrochloric acid, respectively, for the Standard Reference Solution. Using helium as the carrier gas, set the chromatograph gas flow at 2.0 psi constant flow. Use a 0.5-µL injection volume. Set the injection temperature in track mode at 3° above oven temperature, and set the oven temperature to 40° for 6 min and raising it to 280° in 15°-per-min increments over 5 min. Set the detector temperature at 380°. Allow the butyl ester sample phases to separate (centrifugation may be used to hasten the separation). Transfer approximately 1 mL of the hexane layer into an autosampler vial. Run the gas chromatography program. Calculation Determine the response factors (RFi) for butyl ester standards with the equation RFi = 100% × Ai/[Wi × (% purity)i], in which Ai is the average peak area counts for the ith standard; Wi is the weight, in µg, of the ith standard in the Standard Reference Solution; and (%purity)i is the purity of the ith standard expressed as a percentage. Determine the weights of butyl esters in the sample with the formula Wi = Ai/RFi, in which Wi is the weight, in µg, of the ith ester in the sample; Ai is the peak area counts for the ith ester in the sample; and RFi is the response factor for the ith ester standard (average area counts/µg). Determine the weights of fatty acids in the sample with the formula (Wi)fatty acid = (Wi)butyl ester × (MWi)fatty acid/(MWi)butyl ester, in which (Wi)fatty acid and (Wi)butyl ester are, respectively, the weights, in µg, of the ith fatty acid and its butyl ester in the sample, and (MWi)fatty acid and (MWi)butyl ester are their respective molecular weights. Calculate the short/long (S/L) mole ratio with the following equations (mmolesi)fatty acid = (Wi)fatty acid/[1000 × (MWi)fatty acid], S/L mole ratio = ∑i (mmolesi)SCFA/∑i (mmolesi)LCFA,
FCC IV, Supplement 3
in which (Wi)fatty acid is given in µg, (MWi)fatty acid is given in mg/ mmole, and ∑i (mmolesi)SCFA and ∑i (mmolesi)LCFA are the respective sums of the millimoles of short-chain fatty acids (C2– C4) and long-chain fatty acids (C14–C18). Total Saturated LCFAs Using the SCFA/LCFA Mole Ratio Assay method above, calculate the weight percent of saturated LCFAs: 100 × [(Wi)stearic acid) + (Wi)palmitic acid]/WS, in which WS is the weight, in µg, of the sample. Free Fatty Acids Proceed as directed under Free Fatty Acids, Appendix VII, using the following equivalence factor (e) in the formula given in the procedure: Free fatty acids as oleic acid, e = 28.2. Lead Determine as directed under Method II in the Atomic Absorption Spectrophotometric Graphite Furnace Method under the Lead Limit Test, Appendix IIIB, using a 1-g sample. Monoglycerides Determine as directed in the Assay. Peroxide Value Acetic Acid–Chloroform Solution Mix three volumes of acetic acid with two volumes of chloroform. Saturated Potassium Iodide Solution Dissolve excess potassium iodide in freshly boiled water. Excess solid must remain. Store this solution in the dark. Test it daily by adding 0.5 mL to 30 mL of the Acetic Acid–Chloroform Solution, then add 2 drops of starch TS. If the solution turns blue, requiring more than 1 drop of 0.1 N sodium thiosulfate to discharge the color, prepare a fresh solution. Procedure Accurately weigh about 5 g of the sample into a 250-mL Erlenmeyer flask. Add 30 mL of the Acetic Acid–Chloroform Solution, and swirl to dissolve. Add 0.5 mL of the Saturated Potassium Iodide Solution, allow the mixture to stand, shaking it occasionally, for 1 min, and add 30 mL of water. Slowly titrate with 0.01 N sodium thiosulfate, shaking the flask vigorously until the yellow color is almost gone. Add about 0.5 mL of starch TS, and continue the titration, shaking the flask vigorously to release all the iodine from the chloroform layer until the blue color disappears. Perform a blank determination, and make any necessary correction. Calculation Determine the Peroxide Value (PV, milliequivalent peroxide/kg of sample) using the following formula: PV = (S × N × 1000)/W, in which S is the amount, in mL, of 0.01 N sodium thiosulfate; N is the normality of the sodium thiosulfate; and W is the weight, in g, of the sample. Residue on Ignition Determine as directed in Method I, under Residue on Ignition, Appendix IIC, igniting a 2-g sample. Unsaponifiable Matter Calcium Chloride–Diatomaceous Earth Mixture Using a mortar and pestle, grind 1 part anhydrous calcium chloride with 1 part water, and add 3 parts diatomaceous earth, non-acid washed (Celite 545, or equivalent). Grind to a uniform consistency. This mixture may be stored in a covered amber jar for up to 1 month. Potassium Hydroxide–Diatomaceous Earth Mixture (Note: For multiple analyses, prepare in lots of 75 g or more.) Using a
Monographs / Salatrim / 49
mortar and pestle, grind 2 parts potassium hydroxide pellets with 1 part water. Caution: This action generates considerable heat; wear eye protection and gloves. Add 4 parts diatomaceous earth. Grind the mixture to a uniform consistency. It may be stored in a covered amber jar for up to 10 days. Procedure Saponification Place 10 g of Potassium Hydroxide–Diatomaceous Earth Mixture in a 400-mL mortar. Accurately weigh 5 g of the sample (WS), and transfer it to the mortar. Grind the mixture until the sample is uniformly distributed. Add another 10 g of Potassium Hydroxide–Diatomaceous Earth Mixture, and grind to a uniform consistency. Transfer the mixture to a jar. Transfer any residual sample by using the pestle to sweep 5 g of diatomaceous earth along the sides of the mortar and into the jar. Cap the jar securely, and shake until the mixture is uniform. Heat for 20 to 30 min in an oven at 130°. Gravimetric Extraction Transfer the cooled mixture to the mortar, and regrind it for approximately 30 s to a uniform granular consistency. Loosely fit a plug of glass wool into the tip of a glass chromatography column (30 mm id, 30 cm long overall, with a drip tip 5 cm × 8 mm od). Pack the column with 5 g of Calcium Chloride–Diatomaceous Earth Mixture, and transfer the contents of the mortar to the column. Pack to a total height of 50 to 60 mm. Place a 150-mL tared flask under the column. Qualitatively transfer the residue from the mortar to the column with about 25 mL of dichloromethane. Once this solution has percolated into the column bed, add sufficient dichloromethane so that the column bed is wet and a few drops of eluate have been collected in the flask. Charge the column with 150 mL of dichloromethane, and collect the entire volume in the flask (approximately 25 min). Remove the solvent under a stream of nitrogen with gentle heating while the eluate is being collected. Take the contents of the flask to constant weight under vacuum. Determine the weight of the residue (WR). To check for completeness of extraction, add 20 mL of dichloromethane to the column, and collect the eluate in a second tared flask. Evaporate the contents of the second flask to dryness, and examine it for residue. Determine the weight of the residue (WR1), if present. If residue is found, repeat the procedure with an additional 20 mL of dichloromethane. Calculation Use the total residue weight and the weight of the original sample to calculate the percent of unsaponifiable matter: % unsaponifiable matter = [(WR + WR1 + . . .)/WS] × 100. Water Determine by the Karl Fischer Titrimetric Method, Appendix IIB. Packaging and Storage
Store in well-closed containers.
50 /
DL-Serine
/ Monographs
FCC IV, Supplement 3
Revision: Identification test corrected; Heavy Metals (as Pb) specification and determination deleted. DL-Serine
Revision: Identification Test A corrected; Heavy Metals (as Pb) specification and determination deleted. L-Serine
DL-2-Amino-3-hydroxypropanoic Acid
H2C
CH
HO
NH2
C3H7NO3
L-2-Amino-3-hydroxypropanoic Acid
COOH
H 2C
C
HO H
Formula wt 105.09
C3H7NO3
CAS: [302-84-1]
COOH NH2
Formula wt 105.09 CAS: [56-45-1]
DESCRIPTION
DESCRIPTION
White crystals or a crystalline powder. It is soluble in water, but insoluble in alcohol and in ether. It melts with decomposition at about 246° using a closed capillary tube and a bath preheated to 225°. It is optically inactive.
A white, crystalline powder. It is soluble in water, but is insoluble in alcohol and in ether. It melts with decomposition at about 228°.
Functional Use in Foods
Nutrient; dietary supplement.
REQUIREMENTS Identification Heat 5 mL of a 1:1000 solution with 1 mL of triketohydrindene hydrate TS (ninhydrin TS). A bluish purple or purple color is produced. Assay Not less than 98.5% and not more than 101.5% of C3H7NO3, calculated on the dried basis. Lead Not more than 10 mg/kg. Loss on Drying Not more than 0.3%. Residue on Ignition Not more than 0.1%. TESTS Assay Dissolve about 200 mg, accurately weighed, in 3 mL of formic acid and 50 mL of glacial acetic acid. Titrate with 0.1 N perchloric acid in glacial acetic acid, determining the endpoint potentiometrically. Perform a blank determination (see General Provisions), and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 10.51 mg of C3H7NO3. Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Loss on Drying, Appendix IIC Dry at 105° for 3 h. Residue on Ignition, Appendix IIC Ignite 1 g as directed in the general method. Packaging and Storage
Store in well-closed containers.
Functional Use in Foods
Nutrient; dietary supplement.
REQUIREMENTS Identification A. Heat 5 mL of a 1:1000 solution with 1 mL of triketohydrindene hydrate TS (ninhydrin TS). A reddish purple or purple color is produced. B. Dissolve about 500 mg in 10 mL of water, add 200 mg of periodic acid, and heat. The odor of formaldehyde is produced. Assay Not less than 98.5% and not more than 101.5% of C3H7NO3, calculated on the dried basis. Lead Not more than 10 mg/kg. Loss on Drying Not more than 0.3%. Residue on Ignition Not more than 0.1%. Specific Rotation [α]20° D : Between +13.6° and +16.0° after drying; or [α]25° D : Between +13° and +15.6° after drying. TESTS Assay Dissolve about 200 mg, accurately weighed, in 3 mL of formic acid and 50 mL of glacial acetic acid. Titrate with 0.1 N perchloric acid in glacial acetic acid, determining the endpoint potentiometrically. Perform a blank determination (see General Provisions), and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 10.51 mg of C3H7NO3. Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Loss on Drying, Appendix IIC Dry at 105° for 3 h. Residue on Ignition, Appendix IIB Ignite 1 g as directed in the general method. Specific Rotation, Appendix IIB Determine in a solution containing 10 g of a previously dried sample in sufficient 2 N hydrochloric acid to make 100 mL. Packaging and Storage
Store in well-closed containers.
FCC IV, Supplement 3
Monographs / Silicon Dioxide / 51
Revision: Arsenic and Heavy Metals (as Pb) specifications and determinations deleted.
Silicon Dioxide Synthetic Amorphous Silica SiO2
Formula wt 60.08
INS: 551
CAS: [7631-86-9]
DESCRIPTION Silicon Dioxide is an amorphous substance that shows a noncrystalline pattern when examined by X-ray diffraction. It is produced synthetically either by a vapor-phase hydrolysis process, yielding fumed silica, or by a wet process, yielding precipitated silica, silica gel, colloidal silica, or hydrous silica. Fumed silica is produced in essentially an anhydrous state, whereas the wet-process products are obtained as hydrates or contain surface-adsorbed water. Fumed silica occurs as a white, fluffy, nongritty powder of extremely fine particle size and is hygroscopic. The wet-process silicas occur as white, fluffy powders or as white, microcellular beads or granules and are hygroscopic or absorb moisture from the air in varying amounts. All of these forms of Silicon Dioxide are insoluble in water and in organic solvents, but are soluble in hydrofluoric acid and in hot, concentrated solutions of alkalies. Functional Use in Foods Anticaking agent; defoaming agent; carrier; conditioning agent; chillproofing agent in malt beverages; filter aid. REQUIREMENTS Identification A. Place about 5 mg of the sample in a platinum crucible, mix with 200 mg of anhydrous potassium carbonate, and ignite at a red heat for about 10 min over a burner. Cool, dissolve the melt in 2 mL of freshly distilled water, warming if necessary, and slowly add 2 mL of ammonium molybdate TS. A deep yellow color is produced. B. Place 1 drop of the solution from Identification Test A on a filter paper, and evaporate the solvent. Add 1 drop of a saturated solution of o-toluidine in glacial acetic acid, and place the paper over ammonium hydroxide. A greenish blue spot is produced. Assay Fumed silica: not less than 99.0% of SiO2 after ignition; precipitated silica, silica gel, and hydrous silica: not less than 94.0% of SiO2 after ignition. Lead Not more than 5 mg/kg. Loss on Drying Fumed silica: not more than 2.5%; precipitated silica and silica gel: not more than 7.0%; hydrous silica: not more than 70.0%; colloidal silica: not more than 85.0%. Loss on Ignition Fumed silica: not more than 2.0% after drying; silica gel, hydrous silica gel, and precipitated silica: not more than 8.5% after drying. Soluble Ionizable Salts (as Na2SO4) Precipitated silica, silica gel, and hydrous silica: not more than 5.0%.
TESTS Assay Transfer about 1 g of the sample, previously dried at 105° for 2 h and accurately weighed, into a tared platinum crucible, ignite as directed in the test for Loss on Ignition, cool in a desiccator, and weigh to obtain the ignited sample weight (W). Moisten the residue with 3 or 4 drops of alcohol, add 2 drops of sulfuric acid, and then add enough hydrofluoric acid to cover the wetted sample. Evaporate to dryness on a hot plate, using medium heat (95° to 105°), then add 5 mL of hydrofluoric acid, swirl the dish carefully to wash down the sides, and again evaporate to dryness. Ignite the dried residue to a red heat over a Meker burner, cool in a desiccator, and weigh to obtain the residual weight (w). The difference between the ignited sample weight and the residual weight (W – w) represents the weight of SiO2 in the ignited sample. Lead Determine as directed under Lead in the monograph for Calcium Silicate, using the following procedure to develop the Sample Solution: Transfer 5.0 g of the sample into a 250-mL beaker, add 50 mL of 0.5 N hydrochloric acid, cover with a watch glass, and heat slowly to boiling. Boil gently for 15 min, cool, and let the undissolved material settle. Decant the supernatant liquid through a Whatman No. 3 filter paper, or equivalent, into a 100mL volumetric flask, retaining as much as possible of the insoluble material in the beaker. Wash the slurry and beaker with three 10-mL portions of hot water, decanting each washing through the filter into the flask. Finally, wash the filter paper with 15 mL of hot water, cool the filtrate to room temperature, dilute to volume with water, and mix. Loss on Drying, Appendix IIC Dry at 105° for 2 h. Loss on Ignition Transfer into a suitable tared crucible about 1 g of an accurately weighed sample that has been previously dried at 105° for 2 h. Place the crucible in a cold muffle furnace, and bring the temperature to 900° to 1000° during a 1-h period. Ignite at this temperature for 1 h, cool in a desiccator, and weigh. Soluble Ionizable Salts Weigh accurately 5 g of the sample, previously dried at 105° for 2 h, and stir it with 150 mL of water for at least 5 min in a high-speed mixer. Filter with the aid of suction, and wash the mixer and filter with 100 mL of water in divided portions, adding the washings to the filtrate. Dilute the filtrate to 250 mL with water, and determine its conductance with a suitable conductance bridge assembly. The conductance is not greater than that produced by a control containing 250 mg of anhydrous sodium sulfate in each 250 mL. Packaging and Storage
Store in well-closed containers.
52 / Sodium Acid Pyrophosphate / Monographs
Revision: Fluoride test corrected; Heavy Metals (as Pb) specifications and determination deleted. Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limit for this substance: Cadmium, not more than 2 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
FCC IV, Supplement 3
Fluoride Determine on a 2-g sample as directed in Method IV under the Fluoride Limit Test, Appendix IIIB. Insoluble Substances Dissolve 10 g in 100 mL of hot water, and filter through a tared filtering crucible. Wash the insoluble residue with hot water, dry at 105° for 2 h, cool, and weigh. Lead A 10-g sample meets the requirements of the APDC Extraction Method for Lead, Appendix IIIB. Packaging and Storage
Store in tight containers.
Sodium Acid Pyrophosphate Disodium Pyrophosphate; Disodium Dihydrogen Pyrophosphate Na2H2P2O7
Formula wt 221.94 CAS: [7758-16-9]
DESCRIPTION
Revision: Fluoride test corrected; Heavy Metals (as Pb) specification and determination deleted. Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limits for this substance: Cadmium, not more than 2 mg/kg; Lead, not more than 4 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
White, crystalline powder. It is soluble in water. The pH of a 1:100 solution is about 4. It may contain a suitable aluminum and/or calcium salt to control the rate of reaction in leavening systems.
Sodium Metaphosphate, Insoluble
Functional Use in Foods
Insoluble Sodium Polyphosphate; IMP; Maddrell’s Salt
Buffer; leavening agent; sequestrant.
CAS: [50813-16-6] REQUIREMENTS Identification A. A 1:20 solution gives positive tests for Sodium, Appendix IIIA. B. Dissolve 100 mg of the sample in 100 mL of 1.7 N nitric acid. Add 0.5 mL of this solution to 30 mL of quimociac TS. A yellow precipitate does not form. Heat the remaining portion of the sample solution for 10 min at 95°, and then add 0.5 mL of the solution to 30 mL of quimociac TS. A yellow precipitate forms immediately. Assay Not less than 93.0% and not more than 100.5% of Na2H2P2O7. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 0.005%. Insoluble Substances Not more than 1%. Lead Not more than 2 mg/kg. TESTS Assay Dissolve about 500 mg, accurately weighed, in 100 mL of water in a 400-mL beaker. Using a pH meter, adjust the pH of the solution to 3.8 with hydrochloric acid, then add 50 mL of a 1:8 solution of zinc sulfate (125 g of ZnSO4.7H2O dissolved in water, diluted to 1000 mL, filtered, and adjusted to pH 3.8), and allow to stand for 2 min. Titrate the liberated acid with 0.1 N sodium hydroxide until a pH of 3.8 is again reached. After each addition of 0.1 N sodium hydroxide near the endpoint, allow time for any precipitated zinc hydroxide to redissolve. Each mL of 0.1 N sodium hydroxide is equivalent to 11.10 mg of Na2H2P2O7. Arsenic A solution of 1 g in 10 mL of water meets the requirements of the Arsenic Test, Appendix IIIB.
DESCRIPTION It occurs as a white, crystalline powder. It is a high-molecularweight sodium polyphosphate composed of two long metaphosphate chains (NaPO3) that spiral in opposite directions about a common axis. The Na2O/P2O5 ratio is about 1.0. It is practically insoluble in water but dissolves in mineral acids and in solutions of potassium and ammonium (but not sodium) chlorides. The pH of a 1:3 slurry in water is about 6.5. Functional Use in Foods
Emulsifier; sequestrant; texturizer.
REQUIREMENTS Identification A. Finely powder about 1 g of the sample, and add it slowly to 100 mL of a 1:20 solution of potassium chloride while stirring vigorously. A gelatinous mass is formed. B. Mix 500 mg of the sample with 10 mL of nitric acid and 50 mL of water, boil for about 30 min, and cool. The resulting solution gives positive tests for Sodium and for Phosphates, Appendix IIIA. Assay Not less than 68.7% and not more than 70.0% of P2O5. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 0.005%. Lead (See the note at the beginning of this monograph.)
FCC IV, Supplement 3
Monographs / Sodium Phosphate, Dibasic / 53
TESTS
REQUIREMENTS
Assay Transfer about 800 mg of the sample, accurately weighed, into a 400-mL beaker, add 100 mL of water and 25 mL of nitric acid, cover with a watch glass, and boil for 10 min on a hot plate. Rinse any condensate from the watch glass into the beaker, cool the solution to room temperature, transfer it quantitatively to a 500-mL volumetric flask, dilute to volume with water, and mix thoroughly. Pipet 20.0 mL of this solution into a 500-mL Erlenmeyer flask, add 100 mL of water, and heat just to boiling. Add with stirring 50 mL of quimociac TS, then cover with a watch glass, and boil for 1 min in a well-ventilated hood. Cool to room temperature, swirling occasionally while cooling, then filter through a tared, sintered-glass filter crucible of medium porosity, and wash with five 25-mL portions of water. Dry at about 225° for 30 min, cool, and weigh. Each mg of precipitate thus obtained is equivalent to 32.074 µg of P2O5. Arsenic A solution of 1 g in 15 mL of 2.7 N hydrochloric acid meets the requirements of the Arsenic Test, Appendix IIIB. Fluoride Determine on a 1-g sample dissolved in 5 mL of a 1 to 1 hydrochloric acid solution, as directed in Method IV under the Fluoride Limit Test, Appendix IIIB.
Identification A 1:20 solution gives positive tests for Phosphate and for Sodium, Appendix IIIA. Assay Not less than 98.0% of Na2HPO4 after drying. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 0.005%. Insoluble Substances Not more than 0.2%. Lead (See the note at the beginning of this monograph.) Loss on Drying Anhydrous: Not more than 5.0%; dihydrate: between 18.0% and 22.0%. TESTS
Disodium Monohydrogen Phosphate; Disodium Phosphate
Assay Transfer about 6.5 g of the sample, previously dried at 105° for 4 h and accurately weighed, into a 250-mL beaker, add 50.0 mL of 1 N hydrochloric acid and 50 mL of water, and stir until the sample is completely dissolved. Place the electrodes of a suitable pH meter in the solution, and titrate the excess acid with 1 N sodium hydroxide to the inflection point occurring at about pH 4. Record the buret reading, and calculate the volume (A) of 1 N hydrochloric acid consumed by the sample. Continue the titration with 1 N sodium hydroxide until the inflection point occurring at about pH 8.8 is reached, record the buret reading, and calculate the volume (B) of 1 N sodium hydroxide required in the titration between the two inflection points (pH 4 to pH 8.8). When A is equal to or less than B, each mL of the volume A of 1 N hydrochloric acid is equivalent to 142.0 mg of Na2HPO4. When A is greater than B, each mL of the volume 2B + A of 1 N sodium hydroxide is equivalent to 142.0 mg of Na2HPO4. Arsenic A solution of 1 g in 35 mL of water meets the requirements of the Arsenic Test, Appendix IIIB. Fluoride Determine as directed in Method IV under the Fluoride Limit Test, Appendix IIIB, using a 2-g sample. Insoluble Substances Dissolve 10 g in 100 mL of hot water, and filter through a tared filtering crucible (not glass). Wash the insoluble residue with hot water, dry at 105° for 2 h, cool, and weigh. Loss on Drying Determine as directed under Loss on Drying, Appendix IIC, drying at 120° for 4 h.
Na2HPO4 Na2HPO4.2H2O
Packaging and Storage
Packaging and Storage
Store in tight containers.
Revision: Formula, Formula Weight, and CAS Numbers corrected; Fluoride test corrected; Heavy Metals (as Pb) specification and determination deleted. Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limits for this substance: Cadmium, not more than 2 mg/kg; Lead, not more than 4 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
Sodium Phosphate, Dibasic
INS: 339(ii)
Formula wt, anhydrous 141.96 Formula wt, dihydrate 177.99 CAS: anhydrous [7558-79-4] CAS: dihydrate [10028-24-7]
DESCRIPTION Dibasic Sodium Phosphate occurs as a white, crystalline powder or as granules. It may be anhydrous or contain two molecules of water of hydration. The anhydrous form is hygroscopic. Both forms are freely soluble in water and insoluble in alcohol. Functional Use in Foods trient; dietary supplement.
Emulsifier; texturizer; buffer; nu-
Store in tightly closed containers.
54 / Sodium Phosphate, Monobasic / Monographs
Revision: Formula, Formula Weight, and CAS Numbers corrected; Fluoride test corrected; Heavy Metals (as Pb) specification and determination deleted. Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limits for this substance: Cadmium, not more than 2 mg/kg; Lead, not more than 4 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
Sodium Phosphate, Monobasic Monosodium Phosphate; Sodium Biphosphate; Monosodium Dihydrogen Phosphate NaH2PO4 NaH2PO4.H2O
Formula wt, anhydrous 119.98 Formula wt, monohydrate 137.99
INS: 339(i)
CAS: anhydrous [7558-80-7] CAS: monohydrate [10049-21-5]
DESCRIPTION Monobasic Sodium Phosphate is anhydrous or contains one or two molecules of water of hydration and is slightly hygroscopic. The anhydrous form occurs as a white, crystalline powder or granules. The hydrated forms occur as white or transparent crystals or granules. All forms are freely soluble in water, but are insoluble in alcohol. The pH of a 1:100 solution is between 4.1 and 4.7. Functional Use in Foods supplement.
Buffer; emulsifier; nutrient; dietary
FCC IV, Supplement 3
and calculate the volume (A), if any, of 1 N hydrochloric acid consumed by the sample. Continue the titration with 1 N sodium hydroxide until the inflection point occurring at about pH 8.8 is reached, record the buret reading, and calculate the volume (B) of 1 N sodium hydroxide required in the titration between the two inflection points (pH 4 and pH 8.8). Each mL of the volume B – A of 1 N sodium hydroxide is equivalent to 120.0 mg of NaH2PO4. Arsenic A solution of 1 g of sample in 35 mL of water meets the requirements of the Arsenic Test, Appendix IIIB. Fluoride Determine on a 2-g sample as directed in Method IV under the Fluoride Limit Test, Appendix IIIB Insoluble Substances Dissolve 10 g in 100 mL of hot water, and filter through a tared filtering crucible (not glass). Wash the insoluble residue with hot water, dry at 105° for 2 h, cool, and weigh. Loss on Drying Determine as directed under Loss on Drying, Appendix IIC, drying first at 60° for 1 h, then at 105° for 4 h. Packaging and Storage
Store in tightly closed containers.
Revision: Formula, Formula Weight, and CAS Numbers corrected; Assay and Fluoride tests corrected; Heavy Metals (as Pb) specification and determination deleted. Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limits for this substance: Cadmium, not more than 2 mg/kg; Lead, not more than 4 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
Sodium Phosphate, Tribasic REQUIREMENTS
Trisodium Phosphate
Identification A 1:20 solution gives positive tests for Phosphate and for Sodium, Appendix IIIA. Assay Not less than 98.0% and not more than 103.0% of NaH2PO4, after drying. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 0.005%. Insoluble Substances Not more than 0.2%. Lead (See the note at the beginning of this monograph.) Loss on Drying Anhydrous: Not more than 2.0%; monohydrate: between 10.0% and 15.0%; dihydrate: between 20.0% and 25.0%.
Na3PO4 Na3PO4.12H2O
Formula wt, anhydrous 163.94 Formula wt, dodecahydrate 380.12
INS: 339(iii)
CAS: anhydrous [7601-54-9] CAS: dodecahydrate [10101-89-0]
TESTS Assay Transfer about 5 g of the sample, previously dried at 105° for 4 h and accurately weighed, into a 250-mL beaker, add 50.0 mL of 1 N hydrochloric acid and 100 mL of water, and stir until the sample is completely dissolved. Place the electrodes of a suitable pH meter in the solution, and slowly titrate the excess acid, stirring constantly, with 1 N sodium hydroxide to the inflection point occurring at about pH 4. Record the buret reading,
DESCRIPTION Tribasic Sodium Phosphate occurs as white crystals or granules or as a crystalline material. It may be anhydrous or contain 1 to 12 molecules of water of hydration. The formula for a crystalline material is approximately 4(Na3PO4.12H2O)NaOH. It is freely soluble in water, but is insoluble in alcohol. The pH of a 1:100 solution is between 11.5 and 12.0. Functional Use in Foods supplement.
Buffer; emulsifier; nutrient; dietary
FCC IV, Supplement 3
Monographs / Sodium Polyphosphates, Glassy / 55
REQUIREMENTS Identification A 1:20 solution gives positive tests for Sodium and for Phosphate, Appendix IIIA. Assay Anhydrous and Monohydrate (Na3PO4.H2O): Not less than 97.0% of Na3PO4, calculated on the ignited basis; dodecahydrate: not less than 90.0% of Na3PO4, calculated on the ignited basis. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 0.005%. Insoluble Substances Not more than 0.2%. Lead (See the note at the beginning of this monograph.) Loss on Ignition Anhydrous: Not more than 2.0%; monohydrate: between 8.0% and 11.0%; dodecahydrate: between 45.0% and 57.0%. TESTS
Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limits for this substance: Cadmium, not more than 2 mg/kg; Lead, not more than 4 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
Sodium Polyphosphates, Glassy Sodium Hexametaphosphate; Sodium Tetrapolyphosphate; Graham’s Salt INS: 452
CAS: [68915-31-1]
DESCRIPTION
Assay Dissolve an accurately weighed quantity of the sample, equivalent to between 5.5 and 6 g of anhydrous Na3PO4, in 40 mL of water in a 400-mL beaker, and add 100.0 mL of 1 N hydrochloric acid. Pass a stream of carbon dioxide-free air, in fine bubbles, through the solution for 30 min to expel carbon dioxide, covering the beaker loosely to prevent any loss by spraying. Wash the cover and sides of the beaker with a few mL of water, and place the electrodes of a standard pH meter in the solution. Titrate the solution with 1 N sodium hydroxide to the inflection point occurring at about pH 4, then calculate the volume (A) of 1 N hydrochloric acid consumed. Protect the solution from absorbing carbon dioxide from the air, and continue the titration with 1 N sodium hydroxide until the inflection point occurring at about pH 8.8 is reached. Calculate the volume (B) of 1 N sodium hydroxide consumed in the titration. When A is equal to or greater than 2B, each mL of the volume B of 1 N sodium hydroxide is equivalent to 163.9 mg of Na3PO4. When A is less than 2B, each mL of the volume A + B of 1 N sodium hydroxide is equivalent to 163.9 mg of Na3PO4. Arsenic A solution of 1 g in 35 mL of water meets the requirements of the Arsenic Test, Appendix IIIB. Fluoride Determine as directed in Method IV under the Fluoride Limit Test, Appendix IIIB, using a 2-g sample. Insoluble Substances Dissolve 10 g in 100 mL of hot water, and filter through a tared filtering crucible (not glass). Wash the insoluble residue with hot water, dry at 105° for 2 h, cool, and weigh. Loss on Ignition Ignite at about 800° for 30 min after drying at 110° for 5 h. Packaging and Storage
Revision: Fluoride test corrected; Heavy Metals (as Pb) specification and determination deleted.
Store in tightly closed containers.
These substances occur as colorless or white, transparent platelets, granules, or powders. They are a class consisting of several amorphous, water-soluble polyphosphates composed of linear chains of metaphosphate units, (NaPO3)x where x ≥ 2, terminated by Na2PO4, groups. They are usually identified by their Na2O/ P2O5 ratio or their P2O5 content. The Na2O/P2O5 ratios vary from about 1.3 for sodium tetrapolyphosphate, for which x = approximately 4; through about 1.1 for Graham’s salt, commonly called sodium hexametaphosphate, for which x = 13 to 18; to about 1.0 for the higher molecular weight sodium polyphosphates, for which x = 20 to 100 or more. The pH of their solutions varies from about 3.0 to 9.0. The Glassy Sodium Polyphosphates are very soluble in water. Functional Use in Foods
Emulsifier; sequestrant; texturizer.
REQUIREMENTS Identification A. A 1:20 solution gives positive tests for Sodium, Appendix IIIA. B. Dissolve about 100 mg in 5 mL of hot 1.7 N nitric acid, warm on a steam bath for 10 min, and cool. Neutralize to litmus paper with 1 N sodium hydroxide, and add silver nitrate TS. A yellow precipitate is formed that is soluble in 1.7 N nitric acid. Assay Between 60.0% and 71.0% of P2O5. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 0.005%. Insoluble Substances Not more than 0.1%. Lead (See the note at the beginning of this monograph.) TESTS Assay Transfer about 800 mg of the sample, accurately weighed, into a 400-mL beaker, add 100 mL of water and 25 mL of nitric acid, cover with a watch glass, and boil for 10 min on a hot plate. Rinse any condensate from the watch glass into the beaker, cool the solution to room temperature, transfer it quanti-
56 / Sodium Potassium Tripolyphosphate / Monographs
tatively to a 500-mL volumetric flask, dilute to volume with water, and mix thoroughly. Pipet 20.0 mL of this solution into a 500-mL Erlenmeyer flask, add 100 mL of water, and heat just to boiling. Add with stirring 50 mL of quimociac TS, then cover with a watch glass, and boil for 1 min in a well-ventilated hood. Cool to room temperature, swirling occasionally while cooling, then filter through a tared, sintered-glass filter crucible of medium porosity, and wash with five 25-mL portions of water. Dry at about 225° for 30 min, cool, and weigh. Each mg of precipitate thus obtained is equivalent to 32.074 µg of P2O5. Arsenic A solution of 1 g in 35 mL of water meets the requirements of the Arsenic Test, Appendix IIIB. Fluoride Determine on a 2-g sample as directed in Method IV under the Fluoride Limit Test, Appendix IIIB. Insoluble Substances Dissolve 10 g in 100 mL of hot water, and filter through a tared filtering crucible. Wash the insoluble residue with hot water, dry at 105° for 2 h, cool, and weigh. Packaging and Storage
Store in tight containers.
FCC IV, Supplement 3
TESTS Perform the TESTS as described in the monograph for Sodium Tripolyphosphate (in this Supplement). Packaging and Storage
Revision: Fluoride test corrected; Heavy Metals (as Pb) specification and determination deleted. Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limits for this substance: Cadmium, not more than 2 mg/kg; Lead, not more than 4 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
Sodium Trimetaphosphate (NaPO3)3
Sodium Potassium Tripolyphosphate Trisodium Dipotassium Tripolyphosphate Na3K2P3O10
DESCRIPTION Sodium Trimetaphosphate occurs as white crystals or as a white, crystalline powder. It is a cyclic polyphosphate composed of three metaphosphate units. It is freely soluble in water. The pH of a 1:100 solution is about 6.0. Functional Use in Foods
Starch-modifying agent.
REQUIREMENTS Formula wt 400.1 CAS: [24315-83-1]
DESCRIPTION Sodium Potassium Tripolyphosphate occurs as white, slightly hygroscopic granules, or as a powder. It is anhydrous. It is freely soluble in water. The pH of a 1:100 solution is about 10. Functional Use in Foods
Formula wt 305.89 CAS: [7785-84-4]
Revision: Fluoride test corrected; Heavy Metals (as Pb) specification and determination deleted. Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limit for this substance: Cadmium, not more than 2 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
Store in tight containers.
Texturizer; sequestrant.
REQUIREMENTS Identification A 1:20 solution gives positive tests for Sodium, for Potassium, and for Phosphate, Appendix IIIA. Assay Not less than 85.0% and not more than 100.5% of Na3K2P3O10. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 0.005%. Insoluble Substances Not more than 0.1%. Lead Not more than 2 mg/kg.
Identification A. A 1:20 solution gives positive tests for Sodium, Appendix IIIA. B. Dissolve about 100 mg in 5 mL of hot 1.7 N nitric acid, warm on a steam bath for 10 min, and cool. Neutralize to litmus paper with 1 N sodium hydroxide, and add silver nitrate TS. A yellow precipitate is formed that is soluble in 1.7 N nitric acid. Assay Between 68.0% and 70.0% of P2O5. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.) Fluoride Not more than 0.005%. Insoluble Substances Not more than 0.1%. Lead (See the note at the beginning of this monograph.) TESTS Assay Transfer about 800 mg of the sample, accurately weighed, into a 400-mL beaker, add 100 mL of water and 25 mL of nitric acid, cover with a watch glass, and boil for 10 min on a hot plate. Rinse any condensate from the watch glass into the beaker, cool the solution to room temperature, transfer it quantitatively to a 500-mL volumetric flask, dilute to volume with water, and mix thoroughly. Pipet 20.0 mL of this solution into a
FCC IV, Supplement 3
Monographs / Sodium Tripolyphosphate / 57
500-mL Erlenmeyer flask, add 100 mL of water, and heat just to boiling. Add with stirring 50 mL of quimociac TS, then cover with a watch glass, and boil for 1 min in a well-ventilated hood. Cool to room temperature, swirling occasionally while cooling, then filter through a tared, sintered-glass filter crucible of medium porosity, and wash with five 25-mL portions of water. Dry at about 225° for 30 min, cool, and weigh. Each mg of precipitate thus obtained is equivalent to 32.074 µg of P2O5. Arsenic A solution of 1 g in 35 mL of water meets the requirements of the Arsenic Test, Appendix IIIB. Fluoride Determine on a 2-g sample as directed in Method IV under the Fluoride Limit Test, Appendix IIIB. Insoluble Substances Dissolve 10 g in 100 mL of hot water, and filter through a tared filtering crucible. Wash the insoluble residue with hot water, dry at 105° for 2 h, cool, and weigh. Packaging and Storage
Store in tight containers.
Revision: Fluoride test corrected; Heavy Metals (as Pb) specification and determination deleted. Note: The Committee on Food Chemicals Codex is proposing the following additional heavy metal limit for this substance: Cadmium, not more than 2 mg/kg. Manufacturers and users are invited to comment on the proposed limits.
Sodium Tripolyphosphate Pentasodium Triphosphate; Triphosphate; Sodium Triphosphate Na5P3O10 INS: 451(i)
Formula wt 367.86 CAS: [7758-29-4]
DESCRIPTION Sodium Tripolyphosphate occurs as white, slightly hygroscopic granules, or as a powder. It is anhydrous or contains six molecules of water of hydration. It is freely soluble in water. The pH of a 1:100 solution is about 9.5. Functional Use in Foods
Texturizer; sequestrant.
REQUIREMENTS Identification A. A 1:20 solution gives positive tests for Sodium, Appendix IIIA. B. Add a few drops of silver nitrate TS to 1 mL of a 1:100 solution. A white precipitate is formed that is soluble in 1.7 N nitric acid. Assay Anhydrous: not less than 85.0% of Na5P3O10; hexahydrate: not less than 65.0% of Na5P3O10. Arsenic (as As) Not more than 3 mg/kg. Cadmium (See the note at the beginning of this monograph.)
Fluoride Not more than 0.005%. Insoluble Substances Not more than 0.1%. Lead Not more than 2 mg/kg. TESTS Assay Potassium Acetate Buffer (pH 5.0) Dissolve 78.5 g of potassium acetate in 1000 mL of water, and adjust the pH of the solution to 5.0 with glacial acetic acid. Add a few mg of mercuric iodide to inhibit mold growth. 0.3 M Potassium Chloride Solution Dissolve 22.35 g of potassium chloride in water, add 5 mL of Potassium Acetate Buffer, dilute with water to 1000 mL, and mix. Add a few mg of mercuric iodide to inhibit mold growth. 0.6 M Potassium Chloride Solution Dissolve 44.7 g of potassium chloride in water, add 5 mL of Potassium Acetate Buffer, dilute with water to 1000 mL, and mix. Add a few mg of mercuric iodide to inhibit mold growth. 1 M Potassium Chloride Solution Dissolve 74.5 g of potassium chloride in water, add 5 mL of Potassium Acetate Buffer, dilute to 1000 mL with water, and mix. Add a few mg of mercuric iodide to inhibit mold growth. Chromatographic Column Use a standard chromatographic column, 20- to 40-cm long with a 20- to 28-mm id, that has a sealed-in, coarse-porosity, fritted disk. If a stopcock is not provided, attach a stopcock having a 3- to 4-mm diameter bore to the outlet of the column with a short length of flexible vinyl tubing. Procedure Close the column stopcock, fill the space between the fritted disk and the stopcock with water, and connect a vacuum line to the stopcock. Prepare a 1:1 water slurry of Dowex 1 × 8, chloride form, 100- to 200- or 200- to 400-mesh, or a comparable grade of styrene–divinylbenzene ion exchange resin, and decant off any very fine particles and any foam. Do this two or three times or until no more finely suspended material or foaming is observed. Fill the column with the slurry, and open the stopcock to allow the vacuum to pack the resin bed until the water level is slightly above the top of the resin, then immediately close the stopcock. Do not allow the liquid level to fall below the resin level at any time. Repeat this procedure until the packed resin column is 15 cm (about 6 in.) above the fritted disk. Place one circle of tightly fitting glass-fiber filter paper on top of the resin bed, then place a perforated polyethylene disk on top of the paper. Alternatively, a loosely packed plug of glass wool may be placed on top of the bed. Close the top of the column with a rubber stopper in which a 7.6-cm length of capillary tubing (1.5-mm id, 7-mm od) has been inserted through the center, so that about 12 mm of the tubing extends through the bottom of the stopper. Connect the top of the capillary tubing to the stem of a 500-mL separator with flexible vinyl tubing, and clamp the separator to a ring stand above the column. Wash the column by adding 100 mL of water to the separator with all stopcocks closed. First open the separator stopcock, then open the column stopcock. The rate of flow should be about 5 mL/min. When the separator is empty, close the column stopcock, then close the separator stopcock. Transfer about 500 mg of the sample, accurately weighed, into a 250-mL volumetric flask, dissolve and dilute to volume with water, and mix. Transfer 10.0 mL of this solution into the
58 / Solin Oil / Monographs
separator, open both stopcocks, and allow the solution to drain into the column, rinsing the separator with 20 mL of water. Discard the eluate. Add 370 mL of 0.3 M Potassium Chloride Solution to the separator, and allow this solution to pass through the column, discarding the eluate. Add 250 mL of 0.6 M Potassium Chloride Solution to the column, allow the solution to pass through the column, and receive the eluate in a 400-mL beaker. (To ensure a clean column for the next run, pass 100 mL of 1 M Potassium Chloride Solution through the column, and then follow with 100 mL of water. Discard all washings.) Add 15 mL of nitric acid to the beaker, mix, and boil for 15 to 20 min. Add methyl orange TS, and neutralize the solution with ammonium hydroxide. Add 1 g of ammonium nitrate crystals, stir to dissolve, and cool. Add 15 mL of ammonium molybdate TS, with stirring, and stir vigorously for 3 min, or allow to stand with occasional stirring for 10 to 15 min. Filter the contents of the beaker with suction through a 6- to 7-mm paper-pulp filter pad supported in a 25-mm porcelain disk. The filter pad should be covered with a suspension of infusorial earth. After the contents of the beaker have been transferred to the filter, wash the beaker with five 10-mL portions of a 1:100 solution of sodium or potassium nitrate, passing the washings through the filter, then wash the filter with five 5-mL portions of the wash solution. Return the filter pad and the precipitate to the beaker, wash the funnel thoroughly with water into the beaker, and dilute to about 150 mL. Add 0.1 N sodium hydroxide from a buret until the yellow precipitate is dissolved, then add 5 to 8 mL in excess. Add phenolphthalein TS, and titrate the excess alkali with 0.1 N nitric acid. Finally, titrate with 0.1 N sodium hydroxide to the first appearance of the pink color. The difference between the total volume of 0.1 N sodium hydroxide added and the volume of nitric acid required represents the volume, V, in mL, of 0.1 N sodium hydroxide consumed by the phosphomolybdate complex. Calculate the quantity, in mg, of Na5P3O10 in the sample taken by the formula
FCC IV, Supplement 3
This is a new monograph:
Solin Oil Low Linolenic Acid Flaxseed Oil (Unhydrogenated); Low Linolenic Acid Linseed Oil
DESCRIPTION Solin Oil occurs as a light-yellow oil. It is obtained from the seed of certain varieties of the flaxseed plant (Linum usitatissimum L.) by mechanical expression and/or solvent extraction, differing from linseed oil in having a linolenic acid (C18:3) content of less than 5%. The oil is refined, bleached, and deodorized to remove free fatty acids, phospholipids, color, odor and flavor components, and miscellaneous non-oil materials. It is liquid and free from visible foreign material at 21° to 27°, but traces of wax may cause the oil to cloud at refrigeration temperatures (2° to 5°) unless removed by winterization. Functional Use in Foods formulation aid; texturizer.
Coating agent; emulsifying agent;
REQUIREMENTS Identification Low linolenic flaxseed oil exhibits the following composition profile of fatty acids as determined under Fatty Acid Composition, Appendix VII. Fatty Acid:
<14:0 14:0 16:0 16:1 18:0 18:1 18:2
Weight % (Range): <0.1 <0.5 2–9 Fatty Acid:
<0.5 2–5
8–60 40–80
18:3 20:0 20:1 22:0 22:1 24:0
Weight % (Range): <5.0 <0.3 <0.3 <0.3 <0.2 <0.2
0.533 × 25V. Arsenic A solution of 1 g in 35 mL of water meets the requirements of the Arsenic Test, Appendix IIIB. Fluoride Determine on a 2-g sample as directed in Method IV under the Fluoride Limit Test, Appendix IIIB. Insoluble Substances Dissolve 10 g in 100 mL of hot water, and filter through a tared filtering crucible. Wash the insoluble residue with hot water, dry at 105° for 2 h, cool, and weigh. Lead A 10-g sample meets the requirements of the APDC Extraction Method for Lead, Appendix IIIB. Packaging and Storage
Store in tight containers
Cold Test Passes test. Color (AOCS-Wesson) Not more than 5.0 red. Free Fatty Acids (as oleic acid) Not more than 0.1%. Iodine Value Between 100 and 160. Lead Not more than 0.1 mg/kg. Linolenic Acid Not more than 5.0%. Peroxide Value Not more than 10 meq/kg. Unsaponifiable Matter Not more than 1.5%. Water Not more 0.1%. TESTS Cold Test Determine as directed under Cold Test, Appendix VII. Color Determine as directed under Color (AOCS-Wesson), Appendix VII. Free Fatty Acids Determine as directed under Free Fatty Acids, Appendix VII, using the following equivalence factor (e) in the formula given in the procedure: Free fatty acids as oleic acid, e = 28.2.
FCC IV, Supplement 3
Monographs / Soy Protein Concentrate / 59
Iodine Value Determine as directed under Iodine Value, Appendix VII. Lead Determine as directed for the Atomic Absorption Spectrophotometric Graphite Furnace Method, Method II, under the Lead Limit Test, Appendix IIIB, using a 3-g sample. Linolenic Acid Determine as directed under Fatty Acid Composition, Appendix VII. Peroxide Value Determine as directed in Method II under Peroxide Value, Appendix VII. Unsaponifiable Matter Determine as directed under Unsaponifiable Matter, Appendix VII. Water Determine as directed under Water Determination, Appendix IIB. However, in place of 35 to 40 mL of methanol, use 50 mL of chloroform to dissolve the sample. Packaging inert gas.
N sodium hydroxide to the first pink color that persists for at least 30 s. Each mL of 0.1 N sodium hydroxide is equivalent to 11.21 mg of C6H8O2. Melting Range, Appendix IIB Determine as directed for Melting Range or Temperature, Procedure for Class Ia, but heat at a rate of rise of 10°/min until the melting is complete. Residue on Ignition, Appendix IIC Ignite 2 g as directed in the general method. Water Determine by the Karl Fischer Titrimetric Method, Appendix IIB. Packaging and Storage Store in tight containers protected from light, preferably at a temperature not exceeding 38°.
Store in tightly closed containers blanketed in an
This is a new monograph:
Soy Protein Concentrate CAS: [9010-10-0]
Revision: Sample color in Description corrected; Heavy Metals (as Pb) specification and determination deleted.
Sorbic Acid
DESCRIPTION
2,4-Hexadienoic Acid CH3CH CHCH CHCOOH
C6H8O2 INS: 200
Formula wt 112.13 CAS: [110-44-1]
DESCRIPTION A white to off-white, free-flowing powder. It is slightly soluble in water. One g dissolves in about 10 mL of ethanol and in about 20 mL of ether.
Soy Protein Concentrate is derived from soybean (Glycine max) by specific processing steps employed to reduce or remove nonprotein constituents (water, oil, and carbohydrates) to achieve a 65% minimum protein content on the dry basis. It may be in the form of powder, granules, textured flakes, or textured chunks, with color ranging from off-white to tan. Good manufacturing practice requires that the pH during processing not exceed 9 to avoid formation of lysinoalanine. Functional Use in Foods Formulation aid; protein supplement; water and fat binder; stabilizer and thickener; texturizing agent. REQUIREMENTS
Functional Use in Foods
Preservative; mold inhibitor.
REQUIREMENTS Identification A. To 2 mL of a 1:10 solution of the sample in alcohol add a few drops of bromine TS. The color is discharged. B. A 1:400,000 solution in isopropanol exhibits an absorbance maximum at 254 ± 2 nm. Assay Not less than 99.0% and not more than 101.0% of C6H8O2, calculated on the anhydrous basis. Melting Range Between 132° and 135°. Residue on Ignition Not more than 0.2%. Water Not more than 0.5%.
Note: Perform all calculations, except those for Loss on Drying, on the dried basis. Identification Soy Protein Concentrate exhibits the compositional profile specified below with respect to Ash, Fat, Loss on Drying, and Protein. Ash (Total) Not more than 9.0%. Fat Not more than 4.0%. Lead Not more than 1 mg/kg. Loss on Drying Not more than 10.0%. pH of a 10% Suspension Between 5.5 and 7.5. Protein Not less than 65.0% and not more than 89.9%. TESTS
TESTS Assay Dissolve about 250 mg, accurately weighed, in 50 mL of anhydrous methanol that previously has been neutralized with 0.1 N sodium hydroxide, add phenolphthalein TS, and titrate with 0.1
Ash (Total) Proceed as directed in the general method, Appendix IIC, to a final gray to white residue. Fat Proceed as directed in the general method under Crude Fat, Appendix X.
60 / Sucrose Acetate Isobutyrate / Monographs
Lead A sample solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 1 µg of lead ion (Pb) in the control. Loss on Drying Proceed as directed in the general method, Appendix IIC. Dry at 65° at a pressure less than 100 mm of mercury for 16 h using a 2-g sample. Protein Determine the percent of nitrogen as directed in the Nitrogen Determination (Kjeldahl Method), Appendix IIIC, or by the Protein Nitrogen Combustion Method, AOAC 992.23 or AOCS Ba 4e-93. The percent protein equals percent N × 6.25 and is calculated to exclude added vitamins, minerals, amino acids, and food additives. pH of a 10% Suspension Determine by the Potentiometric Method, Appendix IIB, using a 10% solution.
FCC IV, Supplement 3
REQUIREMENTS Identification Identify Sucrose Acetate Isobutyrate by comparing its infrared absorption spectrum with a typical spectrum as shown in the section of Infrared Spectra. Assay Not less than 98.8% and not more than 101.9% of C40H62O19. Acid Value Not more than 0.2. Lead Not more than 1 mg/kg. Saponification Value Not less than 524 and not more than 540. TESTS Assay
Calculate the percentage of C40H62O19 by the formula [(SV × 0.10586)/56.1] × 100,
Packaging and Storage from humidity.
Store in tight containers protected
This is a new monograph:
Sucrose Acetate Isobutyrate SAIB
in which SV is the saponification value. Acid Value Determine as directed in Method I under Acid Value, Appendix VII. Lead Determine as directed for Method II in the Atomic Absorption Spectrophotometric Graphite Furnace Method under the Lead Limit Test, Appendix IIIB. Saponification Value Determine as directed under Saponification Value, Appendix VII. Packaging and Storage
CH2-R1
CH2-R2
O
O R2
R2 O R2
CH2-R1 R2
Revision: Identification Test A corrected; Heavy Metals (as Pb) specification and determination deleted.
R2
L-Threonine
in which R1 = -OOCCH3, and R2 = -OOCCH(CH3)2
C40H62O19
L-2-Amino-3-hydroxybutyric Acid
CH3CHCCOOH HO H NH2
Formula wt 846.9 (range 832–856)
INS: 444
CAS: [27216-37-1] CAS: [123-13-6]
C4H9NO3
DESCRIPTION
Sucrose Acetate Isobutyrate occurs as a clear, pale yellow, viscous liquid. It consists of a mixture of sucrose esters of acetic and isobutyric acid, with sucrose diacetate hexaisobutyrate being the predominant sucrose ester. It is produced through the controlled esterification of sucrose with acetic anhydride and isobutyric anhydride. It is very soluble in essential oils, such as orange oil; soluble in ethanol and in ethyl acetate; and very slightly soluble in water.
L-Threonine
Stabilizer.
Formula wt 119.12 CAS: [72-19-5]
DESCRIPTION
Functional Use in Foods
Store in well-closed containers.
occurs as a white, crystalline powder. It is freely soluble in water, but insoluble in alcohol, in ether, and in chloroform. It melts with decomposition at about 256°.
Functional Use in Foods
Nutrient; dietary supplement.
REQUIREMENTS Identification A. Heat 5 mL of a 1:1000 solution with 1 mL of triketohydrindene hydrate TS (ninhydrin TS). A reddish purple or purple color is produced. B. Add 5 mL of a saturated solution of potassium periodate to 5 mL of a 1:10 solution, and heat. Ammonia is evolved.
FCC IV, Supplement 3
Monographs / Triacetin / 61
Assay Not less than 98.5% and not more than 101.5% of C4H9NO3, calculated on the dried basis. Lead Not more than 10 mg/kg. Loss on Drying Not more than 0.2%. Residue on Ignition Not more than 0.1%. Specific Rotation [α]D20°: Between –26.5° and –29.0° after drying; or [α]25° D : Between –25.8° and –28.8° after drying. TESTS Assay Dissolve about 200 mg, accurately weighed, in 3 mL of formic acid and 50 mL of glacial acetic acid, add 2 drops of crystal violet TS, titrate with 0.1 N perchloric acid to a green endpoint or until the blue color disappears completely. Perform a blank determination (see General Provisions), and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 11.91 mg of C4H9NO3. Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Loss on Drying, Appendix IIC Dry at 105° for 3 h. Residue on Ignition, Appendix IIC Ignite 1 g as directed in the general method. Specific Rotation, Appendix IIB Determine in a solution containing 6 g of a previously dried sample in sufficient water to make 100 mL. Packaging and Storage
Store in well-closed containers.
Revision: Description corrected to show solubility; Heavy Metals (as Pb) specification and determination deleted.
Triacetin Glyceryl Triacetate H HCOOCCH3 HCOOCCH3 HCOOCCH3 H
C9H14O6 INS: 1518
Formula wt 218.21 CAS: [102-76-1]
REQUIREMENTS Identification A. Heat a few drops in a test tube with about 500 mg of potassium bisulfate. Pungent vapors of acrolein are evolved. B. The solution resulting from the Assay gives positive tests for Acetate, Appendix IIIA. Assay Not less than 98.5% of C9H14O6. Acidity Passes test. Refractive Index Between 1.429 and 1.431 at 25°. Specific Gravity Between 1.154 and 1.158. Unsaturated Compounds Passes test. Water Not more than 0.2%. TESTS Assay Transfer about 1 g of the sample, accurately weighed, into a suitable pressure bottle, add 25.0 mL of 1 N potassium hydroxide and 15 mL of isopropanol, stopper the bottle, and wrap securely in a canvas bag. Place in a water bath maintained at 98° ± 2°, and heat for 1 h, allowing the water in the bath to just cover the liquid in the bottle. Remove the bottle from the bath, cool in air to room temperature, then loosen the wrapper, uncap the bottle to release any pressure, and remove the wrapper. Add 6 to 8 drops of phenolphthalein TS, and titrate the excess alkali with 0.5 N sulfuric acid just to the disappearance of the pink color. Perform a blank determination (see General Provisions). Each mL of 0.5 N sulfuric acid is equivalent to 36.37 mg of C9H14O6. Acidity Transfer about 25 g of the sample, accurately weighed, into a 125-mL conical flask, add 50 mL of toluene and 2 drops of thymol blue TS, and titrate rapidly with 0.02 M sodium methoxide in toluene. Swirl the flask continuously until the yellow color changes to a dark color, and then continue the titration without stopping but slowing the addition of titrant until a single drop changes the solution to a clear blue color. The endpoint is stable for about 8 to 15 s. Not more than 1.0 mL of 0.02 M sodium methoxide is required. Refractive Index, Appendix IIB Determine at 25° with an Abbé or other refractometer of equal or greater accuracy. Specific Gravity Determine by any reliable method (see General Provisions). Unsaturated Compounds To 10 mL of the sample in a glassstoppered tube add, dropwise, a solution of bromine in carbon tetrachloride (1 mL in 100 mL) until a permanent yellow color is produced, and allow to stand in a dark place for 18 h. No turbidity or precipitate appears. Water Determine by the Karl Fischer Titrimetric Method, Appendix IIB. Packaging and Storage
DESCRIPTION A colorless, somewhat oily liquid. It is soluble in 14 parts water, and is miscible with alcohol, with ether, and with chloroform. It distills between 258° and 270°. Functional Use in Foods
Humectant; solvent.
Store in well-closed containers.
62 / L-Valine / Monographs
FCC IV, Supplement 3
Revision: Identification test corrected; Heavy Metals (as Pb) specification and determination deleted. L-Valine L-2-Amino-3-methylbutyric Acid
CH3CH CCOOH H3C H C5H11NO2
NH2
TESTS Formula wt 117.15 CAS: [72-18-4]
DESCRIPTION A white, crystalline powder. It is freely soluble in water, but is practically insoluble in alcohol and in ether. The pH of a 1:20 solution is between 5.5 and 7.0. In a closed capillary tube it melts at about 315°. Functional Use in Foods
Assay Not less than 98.5% and not more than 101.5% of C5H11NO2, calculated on the dried basis. Lead Not more than 10 mg/kg. Loss on Drying Not more than 0.3%. Residue on Ignition Not more than 0.1%. Specific Rotation [α]20° D : Between +26.7° and +29.0° after drying; or [α]25° D : Between +26.6° and +28.9° after drying.
Nutrient; dietary supplement.
REQUIREMENTS Identification Heat 5 mL of a 1:1000 solution with 1 mL of triketohydrindene hydrate TS (ninhydrin TS). A reddish purple or bluish color is produced.
Assay Dissolve about 200 mg, accurately weighed, in 3 mL of formic acid and 50 mL of glacial acetic acid, add 2 drops of crystal violet TS, and titrate with 0.1 N perchloric acid to a green endpoint or until the blue color disappears completely. Perform a blank determination (see General Provisions), and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 11.72 mg of C5H11NO2. Lead A Sample Solution prepared as directed for organic compounds meets the requirements of the Lead Limit Test, Appendix IIIB, using 10 µg of lead ion (Pb) in the control. Loss on Drying, Appendix IIC Dry at 105° for 3 h. Residue on Ignition, Appendix IIC Ignite 1 g as directed in the general method. Specific Rotation, Appendix IIB Determine in a solution containing 8 g of a previously dried sample in sufficient 6 N hydrochloric acid to make 100 mL. Packaging and Storage
Store in well-closed containers.
3⁄
Flavor Chemicals
SPECIFICATIONS FOR FLAVOR CHEMICALS Note 5 (Assay) Assay requirements are specified as minimum values (unless a range of assay values is given) and are stated in weight percent unless otherwise indicated. References to assay methods are indicated by citations in parentheses, e.g., “(M1a)” to methods provided under Test Methods for Flavor Chemicals. Note 6 (A.V.) Unless otherwise indicated, determine the acid value (A.V.) as directed in M-16, using phenolphthalein TS as the indicator unless another indicator is specified for an individual substance. Where Method II is specified, determine the acid value as directed in the general method, Appendix VII, Fats and Related Substances. Note 7 (Ref. Index) Refractive index (Ref. Index) determinations are made at 20° unless another temperature is specified, according to the general method, Appendix II, Physical Tests and Determinations. Note 8 (Sp. Gr.) Specific gravity (Sp. Gr.) determinations are made at 25° unless another temperature is specified by any reliable method (see General Provisions). Note 9 (Other Requirements) Numerical limits for other requirements are specified as maximum values unless otherwise indicated (max = maximum; NLT = not lower than or not less than, as appropriate). Test methods are indicated by citations in parentheses, which refer either to methods given in the section that follows this tabular section or to general methods given in Appendix VI, Essential Oils and Flavors.
New and revised specifications for flavor chemicals follow in tabular format. The following Explanatory Notes, given in the Fourth Edition, are unchanged: Explanatory Notes to Tabular Specifications Note 1 (Solubility) Approximate solubilities (see General Provisions) are indicated by the following abbreviations: vs = very soluble; s = soluble; ss = slightly soluble; vss = very slightly soluble; m = miscible; ins = insoluble or practically insoluble. Other abbreviations are as follows: alc = alcohol; gly = glycerin; org = organic; prop = propylene (as in propylene glycol); veg = vegetable (as in vegetable oil); vol = volatile. Note 2 (B.P.) Boiling points (B.P.) are expressed in °C. They are approximate values given for information only and not as requirements. Note 3 (Solubility in Alcohol) Determine the solubility in alcohol at 25° as directed in the general method, Appendix VI, Essential Oils and Flavors. Note 4 (I.D.) The notation “IR” in the identification (I.D.) column indicates that an infrared absorption spectrum is provided for the particular substance in the section entitled Infrared Spectra. Where the IR requirement is specified, the infrared absorption spectrum of the sample shall exhibit maxima at the same wavelengths (or frequencies) as those shown in the respective spectrum, using the test conditions as specified therein.
63
64 / Acetaldehyde Diethyl Acetal / Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Name of Substance Synonyms
Formula Wt/Formula/ Structure
Physical Form/ Odor
Solubility1/ B.P.2
Solubility in Alcohol3
Acetaldehyde Diethyl Acetal This is a new flavor monograph. FEMA No. 2002 Acetal
[insert M2002.eps] 118.17/C 6H14O2/
colorless to pale yel liq/ ethereal, fruity
s—prop glycol, veg oils; ss—water/ 102°
1 mL in 1 mL 95% ethanol
Acetoin Monograph split to monomer and dimer; Ref. Index, Sp. Gr. revised. FEMA No. 2008 Acetyl Methyl Carbinol; Dimethylketol; 3-Hydroxy-2butanone
Monomer [insert M2008.eps] 88.11/C 4H 8 O 2 /
Monomer colorless to pale yel liq/ buttery
Monomer m—alc, prop glycol, water; ins—veg oils/ 148°
H3C HC
O C 2H 5 O C 2H 5
CH3CH(OH)COCH3
Dimer [insert M2008dimer.eps] 176.21/C 8H16O4/ (a) H C 3 HO C HO C H 3C
CH3 C OH C OH CH3
(b)
CH3 HO C O H C O CH3
CH3 C H C OH CH3
2-Acetylpyrrole Color, Melting Range revised; Solubility, Solubility in Alcohol added; Water deleted. FEMA No. 3202 Methyl 2-Pyrrolyl Ketone
[insert M3202.eps] 109.13/C 6H7NO/
2-Acetyl Thiazole This is a new flavor monograph. FEMA No. 3328
127.17/C [insert M3328.eps] 5H5NOS/
N H
Dimer Dimer white to pale yel powder/ s—hot prop glycol; odorless ins—most solvents; ss—weak alkali
white to pale brown fine cryst/ bready
ins—prop glycol, veg oils, water
1 g in 6 mL 95% ethanol
colorless to pale yel liq/ popcorn
s—prop glycol, veg oils; ins—water/ 89° at 12 mm
1 mL in 1 mL 95% ethanol
COCH3
N CH3
S O
Allyl Isothiocyanate Solubility added; B.P. revised. FEMA No. 2034
[insert M2034.eps] 99.16/C 4H5NS/
Allyl Phenoxy Acetate This is a new flavor monograph. FEMA No. 2038
[insert M2038.eps] 192.21/C 11H12O3/
CH2 CH CH2 N C S
colorless to pale yel liq/ honey, pineapple
O O CH2
colorless to pale yel, m—alc, carbon strongly refractive liq/ disulfide, ether/ very pungent irritating 150° odor, acrid taste, mustard (caution: lachrymator)
C O CH2 CH CH2
ss—prop glycol; vss—water; ins—veg oils/ 265°
1 mL in 1 mL 95% ethanol
FCC IV, Supplement 3
Flavor Chemicals / Allyl Phenoxy Acetate / 65
Requirements I.D. Test4
Assay Min. %5
AV Max.6
Ref. Index7
Sp. Gr.8
IR
97.0% of C6H14O2 (M-1b)
1.379–1.384
0.821–0.827
Mon IR
Monomer 96.0% of C4H8O2 (M-1b)
Monomer 1.417–1.422
Monomer 0.995–1.019
Dim IR
Dimer 96.0% of C4H8O2
Other Requirements9
(M-1b)
98.0% of C6H7NO (M-1a)
Melting Range—between 88° and 92° (Appendix IIB) Res. on Ignit.—0.3% (Appendix IIC)
IR
98.0% of C5H5NOS (M-1b)
1.542–1.552
1.219–1.226
IR
93.0% of C3H5NCS (M-1a)
1.527–1.531
1.013–1.020
IR
97.0% of C11H12O3 (M-1b)
1.513–1.518
1.100–1.105
1.0 max
Dist. Range—between 148° and 154° (Appendix IIB) Phenols—passes test (M-18) Allyl Alcohol—NMT 0.1% (M-1b)
66 / Allyl Propionate / Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Name of Substance Synonyms
Formula Wt/Formula/ Structure
Physical Form/ Odor
Solubility1/ B.P.2
Solubility in Alcohol3
Allyl Propionate This is a new flavor monograph. FEMA No. 2040
[insert M2040.eps] 114.15/C 6H10O2/
colorless to pale yel liq/ ethereal, fruity
s—prop glycol, veg oils; ins—water/ 124°
1 mL in 1 mL 95% ethanol
1-Amyl Alcohol Odor revised. FEMA No. 2056 1-Pentanol
[insert M2056.eps] 88.15/C 5H12O/
colorless to pale yel liq/ fusel, winey
m—alc/ 136°
Amyl Butyrate Odor revised. FEMA No. 2059 1-Pentyl Butyrate
158.23/C [insert M2059.eps] 9H18O2/
Amyl Formate Odor revised. FEMA No. 2068 1-Pentyl Formate
116.16/C [insert M2068.eps] 6H12O2/
Borneol This is a new flavor monograph. FEMA No. 2157
O H2C CH CH2 O C C2H5
CH3(CH2)4OH
CH3CH2CH2COOCH2(CH2)3CH3
O CH3(CH2)4OCH
[insert M2157.eps] 154.25/C 10H18O/
H 3C
CH3 CH3 H
colorless to pale yel liq/ fruity, banana
colorless to pale yel liq/ fruity
m—alc/ 128°–130°
white to off-white cryst/ piney, camphoraceous
ss—prop glycol; vss—water; ins—veg oils/ 210°
1 g in 2 mL 95% ethanol
colorless to pale yel liq/ camphoraceous
s—prop glycol, veg oils; ins—water/ 76°at 8 mm
1 mL in 1 mL 95% ethanol
colorless to pale yel liq/ fruity
s—prop glycol, veg oils; ins—water/ 173° at 730 mm
1 mL in 1 mL 95% ethanol
colorless liq/ strong, rancid, butter
m—alc, most fixed oils, prop glycol, water/ 164°
white cryst scales/ honey-floral
s—acetic acid, acetone, benzene, most fixed oils, 1 g in 2000 mL water
OH 2-sec-Butyl Cyclohexanone This is a new flavor monograph. FEMA No. 3261 Freskomenthe
[insert M3261.eps] 154.25/C 10H18O/
Butyl 2-Methyl Butyrate This is a new flavor monograph. FEMA No. 3393
[insert M3393.eps] 158.24/C 9H18O2/
Butyric Acid Sp. Gr. revised; Lead Limit deleted. FEMA No. 2221
88.11/C [insert M2221.eps] 4H8O2/
Cinnamic Acid Solubility in Alcohol revised. FEMA No. 2288 3-Phenylpropenoic Acid
148.16/C [insert M2288.eps] 9H8O2/
O
O C4H9 O C CH C2H5 CH3
CH3(CH2)2COOH
CH CHCOOH
1 g in 7 mL 95% alc
FCC IV, Supplement 3
Flavor Chemicals / Cinnamic Acid / 67
Requirements I.D. Test4 IR
Assay Min. %5 97.0% of C6H10O2 (M-1b)
AV Max.6
Ref. Index7
Sp. Gr.8
2.0 max
1.408–1.413
0.912–0.917
1.407–1.412
0.810–0.816
98.0% of C5H12O (M-1b)
98.0% of C9H18O2 (sum of isomers) (M-1b)
1.0
1.409–1.414
0.863–0.866
92.0% of C6H12O2 (sum of n-, 2-methyl butyl, and 3-methyl butyl isomers) (M-1b)
5.0 add ice to soln
1.396–1.402
0.881–0.887
IR
97.0% of C10H18O (M-1b)
IR
97.0% of C10H18O (sum of 2 isomers) (M-1b)
IR
98.0% of C9H18O2 (M-1b)
IR
99.0% of C4H8O2 (M-3a)
IR
99.0% of C9H8O2 (after drying) (M-3b)
Other Requirements9
Melting Point—202° min.
1.0 max
1.456–1.462
0.910–0.915
1.407–1.413
0.858–0.863
1.397–1.399
0.953–0.957
Reducing Subs.—passes test (M-15)
Melting Range—NLT 130° (Appendix IIB) Res. on Ignit.—0.05% (Appendix IIC)
68 / Cyclohexyl Acetate / Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Name of Substance Synonyms
Formula Wt/Formula/ Structure
Physical Form/ Odor
Solubility1/ B.P.2
Cyclohexyl Acetate Formula Wt, Odor revised. FEMA No. 2349
142.20/C 8H14O2/ [insert M2349.eps]
colorless to pale yel liq/ green, fruity
s—alc/ 174°
colorless to pale yel liq/ kerosene
177°
1 mL in 1 mL 95% alc
yel liq/ powerful, oily, chicken fat
s—alc, fixed oils; ins—water/ 104° (7 mm Hg)
1 mL in 1 mL 95% ethanol
slightly yel liq/ orange, wax
s—alc, most fixed oils; ins—water/ 229°
1 mL in 1 mL 95% ethanol
colorless to slightly yel liq/ orange, fatty
s—alc, most fixed oils; ins—water
1 mL in 1 mL 95% ethanol
almost colorless, oily liq/ spearmint
s—alc, most fixed oils; ins—water/ 225°
1 mL in 1 mL 95% ethanol
almost colorless liq/ herbaceous, spearmint
s—alc, most fixed oils; ins—water/ 222°
1 mL in 1 mL 95% alc
p-Cymene Odor revised. FEMA No. 2356
Solubility in Alcohol3
OCOCH3
134.22/C10H14/ [insert M2356.eps] CH3
CH(CH3)2 (E),(E)-2,4-Decadienal Odor, Solubility revised. FEMA No. 3135 trans,trans-2,4-Decadienal
(E)-2-Decenal Odor, Solubility revised. FEMA No. 2366 trans-2-Decenal (Z)-4-Decenal Odor, Solubility revised. FEMA No. 3264 cis-4-Decenal
152.24/C10H16O/ [insert M3135.eps] CH3(CH2)4 H H C C H C C H CHO 154.25/C10H18O/ [insert M2366.eps] CH3(CH2)6 H C C CHO H
154.25/C 10H18O/ [insert M3264.eps] H
H C C CH3(CH2)4 (CH2)2CHO
1,2-Di[(1'-ethoxy)ethoxy] propane Odor revised. FEMA No. 3534
220.31/C [insert M3534.eps] 11H24O4/
Dihydrocarveol Odor, Solubility revised. FEMA No. 2379
154.25/C [insert M2379.eps] 10H18O/
CH3 CH2 O CH O CH2CH3 CH O CH O CH2CH3 CH3 CH3
CH3 OH
H3C
d-Dihydrocarvone Odor, Solubility in Alcohol, Other Requirements revised. FEMA No. 3565 d-2-Methyl-5-(1-methylethenyl)-cyclohexanone
CH2
154.24/C [insert M3565.eps] 10H16O/ CH3 O
H3C
colorless to pale yel liq/ odorless when pure
CH2
FCC IV, Supplement 3
Flavor Chemicals / d-Dihydrocarvone / 69
Requirements I.D. Test4
Assay Min. %5 98.0% of C8H14O2 (M-1b)
AV Max.6
Ref. Index7
Sp. Gr.8
1.0
1.436–1.441
0.966–0.970
IR
97.0% (M-1a)
1.489–1.491
0.853–0.855
IR
89.0% of C10H16O (sum of two isomers) (M-1a)
1.514–1.519
0.866–0.876
IR
92.0% of C10H18O (one major isomer) (M-1a)
1.452–1.457
0.836–0.846
IR
90.0% of C10H18O (M-1a)
1.442–1.447
0.843–0.850
1.409–1.413
0.915–0.925
96.0% of C10H18O (sum of two isomers) (M-1a)
1.477–1.481
0.921–0.926
92.0% of C10H16O (sum of two isomers) (M-1a)
1.470–1.474
0.923–0.928
97.0% of C11H24O4 (M-1b)
0.1
Other Requirements9
Angular Rotation—between +14° and +22° (Appendix IIB)
70 / Dimethyl Benzyl Carbinyl Butyrate / Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Name of Substance Synonyms
Formula Wt/Formula/ Structure
Physical Form/ Odor
Solubility1/ B.P.2
Solubility in Alcohol3
Dimethyl Benzyl Carbinyl Butyrate Odor, Solubility revised; Angular Rotation deleted. FEMA No. 2394 α,α-Dimethylphenethyl Butyrate
220.31/C [insert M2394.eps] 14H20O2/
almost colorless liq/ prune
s—alc, most fixed oils; ins—prop glycol, water
1 mL in 1 mL 95% ethanol
2,3-Dimethylpyrazine Odor, Solubility revised. FEMA No. 3271
108.14/C 6H8N2/ [insert M3271.eps]
colorless to slightly yel liq/ nutty, cocoa
m—org solvents, water/ 156°
1 mL in 1 mL 95% ethanol
colorless to yellowish oily liq/ burnt
vs—alc, ether; vss—water/ 165°
colorless to pale yel liq/ practically odorless
196°
1 mL in 1 mL 95% alc
colorless to pale yel liq/ disagreeable, intense boiled cabbage
37°
1 mL in 1 mL 95% alc
colorless to white to pale yel liq/ rose
s—veg oils; vss—water/ 259°
1 g in 2 mL 95% ethanol
colorless to yel liq/ coconut-fruity, buttery on dilution
vs—alc, prop glycol, veg oils; ins—water
1 mL in 1 mL 95% ethanol
slightly yel liq/ fatty, citrus
s—alc, most fixed oils; ins—water/ 272°
1 mL in 1 mL 95% ethanol
2,5-Dimethylpyrrole Odor revised.
CH3 CH2COOC(CH2)2CH3 CH3
N
CH3
N
CH3
95.14/C 6H9N/ [insert 25Dimethylpyrrole.eps]
H 3C
N
CH3
H
Dimethyl Succinate Odor revised. FEMA No. 2396
[insert M2396.eps] 146.14/C 6H10O4/
Dimethyl Sulfide B.P. revised. FEMA No. 2746 Methyl Sulfide; Thiobismethane
[insert M2746.eps] 62.14/C 2H6S/
Diphenyl Ether This is a new flavor monograph. FEMA No. 3667 Diphenyl Oxide
170.21/C [insert M3667.eps] 12H10O/
␦-Dodecalactone Solubility revised. FEMA No. 2401
[insert m2401.eps] 198.31/C 12H22O2/
O
O
CH3OC (CH2)2 COCH3
CH3SCH3
O
CH3(CH2)6
(E)-2-Dodecen-1-al Solubility revised. FEMA No. 2402 trans-2-Dodecen-1-al
O
[insert M2402.eps] 182.31/C 12H22O/ CH3(CH2)8 H C C H CHO
O
FCC IV, Supplement 3
Flavor Chemicals / (E)-2-Dodecen-1-al / 71
Requirements I.D. Test4
Assay Min. %5
AV Max.6
Ref. Index7
Sp. Gr.8
Other Requirements9
IR
95.0% of C14H20O2 (M-1b)
1.484–1.489
0.960–0.981
IR
95.0% of C6H8N2
1.506–1.509
1.000–1.022
Dist. Range—between 152° and 157° (Appendix IIB) Solidification Point—between 11° and 13° (Appendix IIB) Tri- and Tetrapyrazines—5% (by GC assay) Water—0.5% (Appendix IIB, KF; use freshly dist. pyridine as solvent)
1.503–1.506
0.932–0.942
Water—0.5% (Appendix IIB, KF; use freshly dist. pyridine as solvent)
1.418–1.421
1.114–1.118
1.431–1.441
0.842–0.847
(M-1a)
IR
98.0% of C6H9N (M-1a)
98.0% of C6H10O4 (M-1b)
IR
99.0% of C2H6S (M-1a)
IR
99.0% of C12H10O (M-1b)
IR
98.0% of C12H22O2 (sum of two isomers; delta isomer 95.0% min) (M-1a)
IR
93.0% of C12H22O (M-1a)
1.0
8.0 (Appendix VII; A.V. Method II)
1.070–1.074
Melting Range—between 26.0° and 30.0°
1.458–1.461
0.942–0.950
Saponification Value—between 278 and 286 (Appendix VI, 1-g sample)
1.454–1.460
0.839–0.849
72 / Ethone / Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Name of Substance Synonyms
Formula Wt/Formula/ Structure
Ethone [insert M2673.eps] 190.24/C 12H14O2/ Odor revised. FEMA No. 2673 CH CHCOCH2CH3 CH3O 1-(p-Methoxyphenyl)-1-penten3-one Ethyl Acetoacetate Odor revised. FEMA No. 2415 Acetoacetic Ester; Ethyl 3Oxybutanoate
130.14/C [insert M2415.eps] 6H10O3/
Ethyl Benzoyl Acetate Odor revised. FEMA No. 2423
[insert M2423.eps] 192.21/C 11H12O3/
Ethyl-(E)-2-butenoate Odor revised. FEMA No. 3486 Ethyl Crotonate; Ethyl-trans2-butenoate
114.14/C [insert M3486.eps] 6H10O2/
Ethylene Brassylate Assay revised. FEMA No. 3543
270.37/C [insert M3543.eps] 15H26O4/
CH3COCH2COOC2H5
Physical Form/ Odor
Solubility1/ B.P.2
white to pale yel cryst/ nutty, maple
Solubility in Alcohol3 1 g in 7 mL 95% alc
colorless to very light yel, mobile liq/ fruity
m—alc, ether, ethyl acetate, 1 mL in 12 mL water/ 181°
light yel liq/ whiskey
265°
colorless to pale yel liq/ ethereal
s—prop glycol; ins—veg oil, water/ 136°
colorless to pale yel liq/ sweet, musky
138°–142° (1 mm Hg) 1 mL in 1 mL 95% alc
colorless to pale yel liq/ green
183°
colorless liq/ cheesy
vs—alc, chloroform, ether, water/ 154°
colorless to pale yel liq/ fruity, apple, green
93°–94° (18 mm Hg)
1 mL in 1 mL 95% alcohol
colorless liq/ strong, green-fruity, apple
s—alc, prop glycol; vss—water; m—most fixed oils/ 133°
1 mL in 1 mL 95% ethanol
CH3C CHCOOC2H5 OH
COCH2CO2CH2CH3
CH3 CH CH COO CH2 CH3
O CH2 C O CH2
1 vol in 1 vol 95% alc
(CH2)9 CH2 C O CH2 O
2-Ethyl Hexanol Odor revised. FEMA No. 3151 2-Ethyl-1-hexanol
130.23/C 8H18O/ [insert M3151.eps]
Ethyl Lactate Odor revised. FEMA No. 2440 Ethyl 2-Hydroxypropionate
118.13/C 5H10O3/ [insert M2440.eps]
Ethyl Levulinate Odor, B.P. revised. FEMA No. 2442
144.17/C 7H12O3/ [insert M2442.eps]
Ethyl 2-Methylbutyrate Odor, Solubility, Ref. Index revised. FEMA No. 2443
130.19/C 7H14O2/ [insert M2443.eps]
CH3(CH2)3CH(C2H5)CH2OH
CH3CHOHCOOC2H5
CH3COCH2CH2COOC2H5
CH3CH2OOCCHCH2CH3 CH3
FCC IV, Supplement 3
Flavor Chemicals / Ethyl 2-Methylbutyrate / 73
Requirements I.D. Test4
Assay Min. %5
AV Max.6
Ref. Index7
Sp. Gr.8
IR
98.0% of C12H14O2 (M-1b)
IR
97.5% of C6H10O3 (M-1b)
5.0 (bromocresol purple TS)
1.418–1.421
1.022–1.027
88.0% of C11H12O3 (M-1b)
2.0
1.528–1.533
1.107–1.120
IR
97.0% of C6H10O2 (M-1b)
5.0
1.422–1.427
0.913–0.920
IR
95.0% of C15H26O4 (M-1a)
1.0
1.468–1.473
1.040–1.045
1.429–1.434
0.830–0.834
Other Requirements9 Solidification Pt.—min. 59.0° (Appendix IIB)
97.0% of C8H18O (M-1b)
IR
98.0% of C5H10O3 (M-1b)
1.0
1.410–1.420
1.029–1.032
IR
98.0% of C7H12O3 (M-1b)
2.0
1.420–1.425
1.007–1.013
95.0% of C7H14O2 (one isomer) (M-1b)
2.0
1.393–1.400
0.863–0.870
74 / Ethyl 2-Methylpentanoate / Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Solubility1/ B.P.2
Solubility in Alcohol3
colorless to pale yel liq/ onion, fruity, sweet
89°–91° (15 mm Hg)
1 mL in 1 mL 95% alc
colorless liq/ wintergreen
s—acetic acid, alc, most fixed oils; ss—gly, water/ 234°
1 mL in 4 mL 80% alc gives clear soln
colorless to pale yel liq/ waxy, coconut
258°–259° (761 mm Hg)
colorless to pale yel liq/ fruity
145°
slightly yel liq/ mild, oily
ins—water/ 263°
1 mL in 1 mL 95% ethanol
colorless to pale yel liq/ camphoraceous
s—prop glycol, veg oils; ins—water/ 192°
1 mL in 1 mL 95% ethanol
white to pale yel cryst/ camphoraceous
s—veg oils; vss—water/ 201°
1 g in 1 mL 95% ethanol
pale yel to brown liq/ caramel
s—prop glycol, veg oils, water/ 169°
1 mL in 1 mL 95% ethanol
yel to brown liq/ coffee
ss—prop glycol, veg oils; vss—water/ 67° at 10 mm
1 mL in 2 mL 95% ethanol
Name of Substance Synonyms
Formula Wt/Formula/ Structure
Physical Form/ Odor
Ethyl 2-Methylpentanoate Odor revised. FEMA No. 3488
144.21/C [insert M3488.eps] 8H16O2/
colorless to pale yel liq/ fruity
Ethyl 3-Methylthiopropionate Odor, Assay revised. FEMA No. 3343
148.23/C [insert M3343.eps] 6H12O2S/
Ethyl Salicylate Odor, Ref. Index revised. FEMA No. 2458
166.18/C 9H10O3/ [insert M2458.eps]
CH3CH2CH2CH(CH3)CO2CH2CH3
CH3SCH2CH2COOCH2CH3
COOC2H5 OH
Ethyl 10-Undecenoate Odor revised. FEMA No. 2461
212.33/C [insert M2461.eps] 13H24O2/
Ethyl Valerate Odor revised. FEMA No. 2462 Ethyl n-Pentanoate
[insert M2462.eps] 130.19/C 7H14O2/
Farnesol Solubility revised. FEMA No. 2478 3,7,11-Trimethyl-2,6,10dodecatrien-1-ol
[insert M2478.eps] 222.37/C 15H26O/
d-Fenchone This is a new flavor monograph. FEMA No. 2479
[insert M2479.eps] 152.24/C 10H16O/
H2C CH(CH2)8CO2C2H5
CH3(CH2)3COOCH2CH3
H 3C
OH CH3
CH3
CH3
CH3 O CH3 CH3
Fenchyl Alcohol This is a new flavor monograph. FEMA No. 2480
154.25/C [insert M2480.eps] 10H18O/ CH3 OH CH3 CH3
Furfuryl Alcohol This is a new flavor monograph. FEMA No. 2491
[insert M2491.eps] 98.10/C 5H6O2/
2-Furyl Methyl Ketone This is a new flavor monograph. FEMA No. 3163
[Insert M3163.eps] 110.11/C 6H6O2/
O
CH2OH
O O
CH3
FCC IV, Supplement 3
Flavor Chemicals / 2-Furyl Methyl Ketone / 75
Requirements I.D. Test4
Assay Min. %5 98.0% of C8H16O2 (M-1b)
AV Max.6
Ref. Index7
Sp. Gr.8
1.0
1.401–1.404
0.859–0.865
1.457–1.463
1.030–1.035
IR
99.0% of C6H12O2S (M-1b)
IR
99.0% of C9H10O3 (M-1b)
1.0 (phenol red TS)
1.520–1.525
1.126–1.130
98.0% of C13H24O2 (M-1b)
1.0
1.436–1.440
0.877–0.879
98.0% of C7H14O2 (M-1b)
1.0
1.399–1.404
0.870–0.875
IR
96.0% of C15H26O (sum of four isomers) (M-1a)
1.487–1.492
0.884–0.891
IR
97.0% of C10H16O (M-1b)
1.460–1.467
0.940–0.948
IR
97.0% of C10H18O (M-1b)
IR
95.0% of C5H6O2 (M-1b)
1.481–1.490
1.126–1.136
IR
97.0% of C10H6O2 (M-1b)
1.505–1.510
1.102–1.107
Other Requirements9
Angular Rotation—between –68° and –46°
Melting Point—between 35.0° and 40.0°
76 / Fusel Oil, Refined / Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Physical Form/ Odor
Solubility1/ B.P.2
Solubility in Alcohol3
colorless to pale yel liq/ winey, whiskey
128°–130°
1 mL in 1 mL 95% alc
slightly yel liq/ fatty, green
s—alc, most fixed oils; ins—water
1 mL in 1 mL 95% ethanol
colorless to slightly yel liq/ penetrating, oily
ss—water; m—alc, ether, fixed oils/ 153°
1 mL in 2 mL 70% alc gives clear soln
colorless, mobile liq/ fruity, spicy
m—alc, ether, 1 mL in 250 mL water/ 151°
slightly yel liq/ fatty, green
s—alc, most fixed oils; ins—water
1 mL in 1 mL 95% ethanol
pale yel liq/ strong, fruity-green, vegetable
s—alc, most fixed oils, prop glycol; vss—water/ 47° (17 mm Hg)
1 mL in 1 mL 95% ethanol
(Z)-3-Hexenyl Isovalerate [insert M3498.eps] 184.28/C 11H20O2/ Odor, Solubility, Sp. Gr. revised. H H FEMA No. 3498 C C cis-3-Hexenyl Isovalerate (CH2)2OOCCH2CH(CH3)2 CH3CH2
colorless liq/ sweet, apple
s—alc, most fixed oils, prop glycol; ins—water/ 199°
1 mL in 1 mL 95% ethanol
(Z)-3-Hexenyl 2-Methylbutyrate [insert M3497.eps] 184.28/C 11H20O2/ Odor, Solubility, Assay revised. H H FEMA No. 3497 C C cis-3-Hexenyl 2(CH2)2OOCCHCH2CH3 CH3CH2 Methylbutyrate CH3
almost colorless liq/ powerful, fruity, unripe apples
s—alc, most fixed oils; ins—water
1 mL in 1 mL 95% ethanol,
Hexyl Alcohol Assay revised. FEMA No. 2567 1-Hexanol; Alcohol C-6
colorless, mobile liq/ mild, sweet, green
m—alc, ether, 1 mL in 175 mL water/ 157°
Name of Substance Synonyms
Formula Wt/Formula/ Structure
Fusel Oil, Refined Odor revised. FEMA No. 2497 (E),(E)-2,4-Heptadienal Solubility revised. FEMA No. 3164 trans,trans-2,4-Heptadienal
110.16/C 7H10O/ [insert M3164.eps] CH3CH2
H H
C C H
C C H
CHO
Heptanal Sp. Gr. revised. FEMA No. 2540 Aldehyde C-7; Heptaldehyde
114.19/C [insert M2540.eps] 7H14O/
2-Heptanone Specific Gravity revised. FEMA No. 2544 Methyl Amyl Ketone
114.19/C [insert M2544.eps] 7H14O/
(Z)-4-Hepten-1-al Solubility revised. FEMA No. 3289 cis-4-Hepten-1-al
[insert M3289.eps] 112.17/C 7H12O/
(E)-2-Hexen-1-al Odor, Solubility revised. FEMA No. 2560 trans-2-Hexen-1-al
[insert M2560.eps] 98.14/C 6H10O/
CH3(CH2)5CHO
CH3CO(CH2)4CH3
H
H C C
CH3CH2
(CH2)2CHO
CH3(CH2)2
H C C
H
[insert M2567.eps] 102.18/C 6H14O/ CH3(CH2)4CH2OH
CHO
FCC IV, Supplement 3
Flavor Chemicals / Hexyl Alcohol / 77
Requirements I.D. Test4
Assay Min. %5
AV Max.6
Ref. Index7
Sp. Gr.8
Other Requirements9 Angular Rotation—between –0.5° and –2.0° (Appendix IIB)
IR
95.0% of 2- and 3methyl butanol (M-1a)
1.405–1.410
0.807–0.813
IR
92.0% of C7H10O (sum of isomers) (M-1a)
1.531–1.537
0.878–0.888
IR
92.0% of C7H14O (M-1b)
10.0
1.412–1.420
0.815–0.820
IR
95.0% of C7H14O (M-1b)
2.0
1.405–1.411
0.811–0.816
IR
98.0% of C7H12O [sum of two isomers; (Z)-4 isomer 93.0% min] (M-1a)
1.432–1.436
0.843–0.855
92.0% of C6H10O (M-1a)
1.445–1.449
0.841–0.850
95.0% of C11H20O2 2.0 [sum of two isomers; (Z) isomer 92.0% min] (M-1a)
1.429–1.435
0.872–0.877
95.0% of C11H20O2 [sum of two isomers; (Z) 92.0% min] (M-1a)
2.0
1.430–1.434
0.876–0.880
97.0% of C6H14O (M-1b)
2.0
1.415–1.420
0.816–0.821
IR
Dist. Range—between 147° and 154° (Appendix IIB) Res. of Evap.—5 mg/100 mL (M-17, 100-mL sample) Water—0.3% (Appendix IIB, KF; use freshly dist. pyridine as solvent)
78 / Hexyl Isovalerate / Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Name of Substance Synonyms
Formula Wt/Formula/ Structure
Physical Form/ Odor
Solubility1/ B.P.2
Hexyl Isovalerate Solubility in Alcohol revised. FEMA No. 3500
186.29/C [insert M3500.eps] 11H22O2/
colorless liq/ jasmine
s—alc, most fixed 1 mL in 1 mL oils; 95% alc ins—gly, prop glycol/ 215°
Hexyl 2-Methylbutyrate Solubility revised. FEMA No. 3499
[insert M3499.eps] 186.29/C 11H22O2/
colorless liq/ strong, fresh-green, fruity
s—alc, most fixed oils; ins—water
colorless to pale yel liq/ winey
m—alc/ 130°
colorless to pale yel liq/ pungent fruit
261° (746 mm Hg)
1 mL in 1 mL 95% alc
colorless liq/ fruity
s—alc, most fixed oils; ins—gly, prop glycol, water/ 179°
1 mL in 4 mL 70% alc
colorless to pale yel liq/ chocolate, honey
268°
1 mL in 1 mL 95% alc
colorless liq/ floral
m—alc, chloroform, ether, most fixed oils; ins—gly, prop glycol, water/ 277°
1 mL in 3 mL 90% alc remains in soln on dilution
colorless liq/ sweet, fruity, balsamic
m—alc, chloroform, ether, most fixed oils; ins—water/ 271°
1 mL in 3 mL 80% alc gives clear soln
colorless, mobile liq/ sharp, pungent
m—alc, ether, 1 mL in 125 mL water/ 64°
(CH3)2CHCH2COOCH2(CH2)4CH3
CH3(CH2)5OOCCHCH2CH3
Solubility in Alcohol3
1 mL in 1 mL 95% ethanol
CH3
Isoamyl Alcohol Odor revised. FEMA No. 2057
88.15/C [insert M2057.eps] 5H12O/
Isoamyl Benzoate Solubility in Alcohol revised. FEMA No. 2058
196.26/C 12H16O2/ [insert M2058.eps]
Isoamyl Butyrate Assay, Ref. Index, Sp. Gr. revised. FEMA No. 2060
158.24/C [insert M2060.eps] 9H18O2/
Isoamyl Phenyl Acetate Odor revised. FEMA No. 2081
206.29/C 13H18O2/ [insert M2081.eps]
Isoamyl Salicylate Odor revised. FEMA No. 2084 Amyl Salicylate
208.26/C 12H16O3/ [insert M2084.eps]
Isobutyl Cinnamate Assay revised. FEMA No. 2193
204.27/C 13H16O2/ [insert M2193.eps]
(CH3)2CHCH2CH2OH
CH2OOCCH2CH(CH3)2
CH3(CH2)2COOCH2CH2CH(CH3)2
CH2COOCH2CH2CH(CH3)2
OH COOCH2CH2CH(CH3)2
CH CHCOOCH2CHCH3 CH3
Isobutyraldehyde Assay revised. FEMA No. 2220
72.11/C 4H8O/ [insert M2220.eps] (CH3)2CHCHO
FCC IV, Supplement 3
Flavor Chemicals / Isobutyraldehyde / 79
Requirements I.D. Test4
AV Max.6
Ref. Index7
Sp. Gr.8
95.0% of C11H22O2 (sum of two isomers; isovalerate isomer 92.0% min) (M-1b)
2.0
1.417–1.421
0.853–0.857
95.0% of C11H22O2 (one isomer) (M-1a)
2.0
1.416–1.421
0.854–0.859
98.0% of C5H12O (sum of 2-methyl butyl, 3-methyl butyl, and npentyl isomers) (M-1b)
1.405–1.410
0.807–0.813
IR
98.0% of C12H16O2 1.0 (sum of 2-methyl butyl, 3-methyl butyl, and n-pentyl isomers) (M-1b)
1.492–1.496
0.986–0.992
IR
98.0% of C9H18O2 1.0 (sum of 2-methyl butyl, 3-methyl butyl, and n-pentyl isomers) (M-1b)
1.409–1.414
0.861–0.866
IR
98.0% of C13H18O2 1.0 (sum of 2-methyl butyl, 3-methyl butyl, and n-pentyl isomers) (M-1b)
1.485–1.490
0.975–0.981
IR
98.0% of C12H16O3 (sum of 2-methyl butyl, 3-methyl butyl, and n-pentyl isomers) (M-1b)
1.0 (phenol red TS)
1.505–1.509
1.047–1.053
IR
98.0% of C13H16O2 (sum of two isomers) (M-1b)
1.0
1.539–1.541
1.001–1.004
IR
98.0% of C4H8O (M-1b)
5.0 (methyl red TS)
Assay Min. %5
0.783–0.788
Other Requirements9
80 / Isopropyl Acetate / Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Name of Substance Synonyms
Formula Wt/Formula/ Structure
Physical Form/ Odor
Solubility1/ B.P.2
Isopropyl Acetate Odor revised. FEMA No. 2926
102.13/C [insert M2926.eps] 5H10O2/
colorless, mobile liq/ ethereal
m—alc, ether, fixed oils, 1 g in 72 mL water/ 88°
Levulinic Acid Odor revised. FEMA No. 2627
116.12/C 5H8O3/ [insert M2627.eps]
yel to brown liq; may congeal/ smoky, caramel
245°
l-Limonene Other Requirements revised. l-p-Mentha-1,8-diene
136.24/C 10H16/ [insert L_Limonene.eps]
colorless liq/ refreshing, light, clean
m—alc, most fixed oils; ins—water/ 177°
Colorless, hexagonal crysts, usually needlelike; fused masses or cryst powder/ pleasant, peppermint
vs—alc, vol oils; ss—water/ 212°
1 mL in 1 mL 95% ethanol
almost colorless liq/ mint
s—alc, most fixed oils; vss—water/ 207°
1 mL in 1 mL 95% ethanol
colorless liq/ mild, minty
s—alc, most fixed oils, prop glycol; ss—water, gly
1 mL in 1 mL 95% ethanol
colorless liq/ mild, minty
s—alc, most fixed oils, prop glycol; ss—water
CH3COOCH(CH3)2
CH3COCH2CH2COOH
CH3
Solubility in Alcohol3
1 mL in 1 mL 95% alc
C H2C
CH3
Menthol Odor, Physical Form, Solubility revised. FEMA No. 2665 3-p-Menthanol (NOTE: l-Menthol is obtained from natural sources or by synthetic processes; dl-Menthol is produced synthetically)
156.27/C 10H20O/ [insert M2665.eps]
l-Menthone Odor, Solubility revised. FEMA No. 2667 l-p-Menthan-3-one
154.25/C 10H18O/ [insert M2668.eps]
OH CH3 CH CH3
H3C
CH3
O H3C
dl-Menthyl Acetate Sp. Gr. revised; Solubility in Alcohol added. FEMA No. 2668 dl-p-Menthan-3-yl Acetate
198.31/C 12H22O2/ [insert M2668.eps] CH3
OOCCH3 H3C
l-Menthyl Acetate Sp. Gr., Other Requirements revised. FEMA No. 2668 l-p-Menthan-3-yl Acetate
CH3
CH3
[insert M2668.eps 198.31/C 12H22O2/ (again)]
CH3
OOCCH3 H3C
CH3
FCC IV, Supplement 3
Flavor Chemicals / l-Menthyl Acetate / 81
Requirements I.D. Test4
Assay Min. %5
AV Max.6
Ref. Index7
2.0
Sp. Gr.8
Other Requirements9
IR
99.0% of C5H10O2 (M-1b)
0.866–0.869
IR
97.0% of C5H8O3 (M-3a)
1.440–1.445
1.136–1.142
Solidification Pt.—min. 27° (Appendix IIB)
95.0% of C10H16 (M-1a)
1.469–1.473
0.837–0.841
Angular Rotation—between –100° and –60° (Appendix IIB, 100-mm tube)
IR
Peroxide Value—5.0 (M-12) Melting Range (l-menthol)—between 41° and 44° (App. IIB) Nonvol. Res.—0.05% (M-17) Readily Ox. Subs. (dl-menthol)—passes test (M-14) Spec. Rotat. (l-menthol)—between –45° and –51° (App. IIB) Spec. Rotat. (dl-menthol)—between –2° and +2° (App. IIB) 96.0% of C10H18O (sum of two isomers) (M-1b)
1.0
1.448–1.453
0.888–0.895
97.0% of C12H22O2 (sum of two isomers) (M-1b)
2.0
1.443–1.450
0.921–0.926
98.0% of C12H22O2 (one major isomer) (M-1b)
2.0
1.443–1.447
0.921–0.926
Angular Rotation—min. –20° (Appendix IIB, 100-mm tube)
Angular Rotation—between –75° and –69° (Appendix IIB, 100-mm tube)
82 / 2-Methoxy-3(5)-methylpyrazine / Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Name of Substance Synonyms
Formula Wt/Formula/ Structure
124.14/C 2-Methoxy-3(5)-methylpyrazine [insert M3183.eps] 6H8N2O/ Odor, Solubility revised. N OCH3 FEMA No. 3183 N
Physical Form/ Odor
Solubility1/ B.P.2
Solubility in Alcohol3
colorless liq/ roasted, hazelnut
s—org solvents, water
1 mL in 1 mL 95% ethanol
colorless to pale yel liq/ chocolate
93°
colorless to pale yel liq/ chocolate
93°
CH3
2-Methyl Butanal Odor revised. FEMA No. 2691
[insert M2691.eps] 86.13/C 5H10O/
3-Methyl Butanal Odor revised. FEMA No. 2692
86.13/C [insert M2692.eps] 5H10O/
2-Methylbutyl Acetate Odor revised. FEMA No. 3644
[insert M3644.eps] 130.18/C 7H14O2/
2-Methylbutyl Isovalerate FEMA Number revised. FEMA No. 3506 2-Methylbutyl-3methylbutanoate
[insert M3506.eps] 172.27/C 10H20O2/
Methyl Butyrate Odor revised. FEMA No. 2693
102.13/C [insert M2693.eps] 5H10O2/
2-Methylbutyric Acid Odor revised. FEMA No. 2695
102.13/C [insert M2695.eps] 5H10O2/
CH3CH2CH(CH3)CHO
(CH3)2CHCH2CHO
CH3CH2CH(CH3)CH2OOCCH3
CH3
colorless to pale yel liq/ banana
colorless liq/ herbaceous, fruity
s—alc, most fixed oils; ins—water
colorless liq/ fruity
102°
colorless to pale yel liq/ fruity
176°
CH3CH2CHCH2OOCCH2CH(CH3)2
CH3(CH2)2COOCH3
CH3CH2CHCOOH
1 mL in 1 mL 95% alc
CH3
Methyl Ionones Structure added; Odor, Solubility revised. Mixture of α-, β-, γ- or α-iso, and δ-isomers
206.3/C [insert METHYLIO.eps] 14H22O/
Methyl Isobutyrate Odor revised. FEMA No. 2694
[insert M2694.eps] 102.13/C 5H10O2/
O
clear to pale yel to yel liq/ woody, orris
1 mL in 1 mL 95% ethanol
(α-iso)
CH3COOCH(CH3)2
Methyl-3-methylthiopropionate [insert M2720.eps] 134.19/C 5H10O2S/ Odor, B.P. revised. CH3SCH2CH2CO2CH3 FEMA No. 2720
colorless liq/ fruity
90°
colorless to pale yel liq/ onion
74°–75° (13 mm Hg)
1 mL in 1 mL 95% alc
FCC IV, Supplement 3
Flavor Chemicals / Methyl-3-methylthiopropionate / 83
Requirements I.D. Test4 IR
IR
Assay Min. %5
AV Max.6
99.0% of C6H8N2O (sum of two isomers) (M-1b)
Ref. Index7
Sp. Gr.8
1.506–1.510
1.070–1.090
97.0% of C5H10O (M-1b)
10.0
1.388–1.393
0.799–0.804
97.0% of C5H10O (M-1b)
10.0
1.388–1.391
0.795–0.802
97.0% of C7H14O2 (M-1b)
1.0
1.399–1.404
0.872–0.877
98.0% of C10H20O2 (M-1a)
2.0
1.413–1.416
0.852–0.857
98.0% of C5H10O2 (M-1b)
1.0
1.386–1.390
0.892–0.897
1.404–1.408
0.932–0.936
98.0% of C5H10O2 (M-3a)
88.0% of C14H22O (sum of four isomers) (M-1b)
5.0
1.497–1.507
0.925–0.934
IR
97.0% of C5H10O2 (M-1b)
1.0
1.382–1.386
0.884–0.888
IR
97.0% of C5H10O2S (M-1a)
1.0
1.462–1.468
1.069–1.078
Other Requirements9
84 / 4-Methyl-2-pentanone / Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Name of Substance Synonyms
Formula Wt/Formula/ Structure
Physical Form/ Odor
Solubility1/ B.P.2
4-Methyl-2-pentanone Ref. Index revised. FEMA No. 2731 Methyl Isobutyl Ketone
100.16/C [insert M2731.eps] 6H12O/
colorless, mobile liq/ fruity, ethereal
m—alc, ether, 1 mL in 50 mL water/ 117°
2-Methyl Propyl 3-Methyl Butyrate Structure, Odor revised. FEMA No. 3369 Isobutyl Isovalerate
158.24/C [insert M3369.eps] 9H18O2/
colorless to pale yel liq/ fruity
m—alc/ 170°
4-Methyl-5-thiazole Ethanol Odor revised. FEMA No. 3204 Sulfurol
143.20/C 9H9NOS/ [insert M3204.eps]
colorless to pale yel liq; may darken upon aging/ meaty
135° (7 mm Hg)
colorless to strawcolored liq/ faint, floral, rose, apple
s—most fixed oils, prop glycol; ins—gly/ 276°
1 mL in 4 mL 70% alc
slightly yel liq/ strong, fatty, floral
s—alc, most fixed oils; ins—water/ 97° (10 mm Hg)
1 mL in 1 mL 95% ethanol
slightly yel liq/ powerful, violet, cucumber
s—alc, most fixed oils; ins—water/ 94° (18 mm Hg)
1 mL in 1 mL 95% ethanol
white to yellowish liq/ powerful, green, vegetable
ins—water/ 196°
1 mL in 1 mL 95% ethanol
colorless to pale yel liq/ fatty
254°
white to slightly yellowish liq/ fatty, violet
s—alc, most fixed oils; ins—water/ 88° (12 mm Hg)
CH3COCH2CH(CH3)2
(CH3)2CHCH2COOCH2CH(CH3)2
H3 C N HOCH2H2C
S
Nerolidol Assay, Formula Wt, Odor revised. FEMA No. 2772 3,7,11-Trimethyl-1,6,10dodecatrien-3-ol
222.37/C 15H26O/ [insert M2772.eps]
(E),(E)-2,4-Nonadienal Solubility revised. FEMA No. 3212 trans,trans-2,4-Nonadienal
138.21/C 9H14O/ [insert M3212.eps]
OH
H CH3(CH2)3 C C H C C H H CHO
(E),(Z)-2,6-Nonadienal Solubility, Assay revised. FEMA No. 3377 trans,cis-2,6-Nonadienal
138.21/C 9H14O/ [insert M3377.eps]
(E),(Z)-2,6-Nonadienol Solubility revised. FEMA No. 2780 trans,cis-2,6-Nonadienol
[insert M2780.eps] 140.22/C 9H16O/
Nonanoic Acid Odor revised. FEMA No. 2784
[insert M2784.eps] 158.24/C 9H18O2/
(E)-2-Nonenal Solubility, Sp. Gr. revised. FEMA No. 3213 trans-2-Nonenal
[insert M3213.eps] 140.22/C 9H16O/
H
H
H
H
H
CH2CH2
H
H C C
C C CH3CH2
CHO C C
C C CH3CH2
Solubility in Alcohol3
CH2CH2
CH3(CH2)7COOH
H CH3(CH2)5 C C CHO H
CH2OH H
1 mL in 1 mL 95% ethanol
FCC IV, Supplement 3
Flavor Chemicals / (E)-2-Nonenal / 85
Requirements I.D. Test4
AV Max.6
Ref. Index7
Sp. Gr.8
Other Requirements9
99.0% of C6H12O (M-2d)
2.0 (M-16)
1.392–1.397
0.796–0.799
Dist. Range—between 114° and 117° (Appendix IIB) Water—0.1% (Appendix IIB, KF; use freshly dist. pyridine as solvent)
98.0% of C9H18O2 (M-1b)
1.0
1.404–1.408
0.850–0.854
98.0% of C9H9NOS (M-1b)
1.548–1.552
1.196–1.210
IR
97% of C15H26O (sum of two isomers) (M-1b)
1.478–1.483
0.870–0.880
IR
89.0% of C9H14O (one major isomer) (M-1a)
1.517–1.523
0.865–0.880
IR
96.0% of C9H14O (sum of two isomers; 90.0% major isomer) (M-1a)
1.470–1.475
0.850–0.870
IR
92.0% of C9H16O (one major isomer) (M-1a)
1.464–1.471
0.860–0.880
98.0% of C9H18O2 (M-3a)
1.431–1.435
0.901–0.906
92.0% of C9H16O (one major isomer) (M-1a)
1.450–1.460
0.840–0.850
IR
Assay Min. %5
Angular Rotation (Natural)—between +11° and +14° (Appendix IIB; 100-mm tube) Esters—0.5% as nerolidyl acetate (Appendix VI; 10 g/132.7)
86 / (E)-2-Nonen-1-ol / Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Name of Substance Synonyms
Formula Wt/Formula/ Structure
Physical Form/ Odor
Solubility1/ B.P.2
Solubility in Alcohol3
(E)-2-Nonen-1-ol Solubility revised. FEMA No. 3379 trans-2-Nonenol
142.24/C [insert M3379.eps] 9H18O/
white liq/ fatty, violet
ins—water
1 mL in 1 mL 95% ethanol
white to slightly yel liq/ powerful, melon
ins—water
1 mL in 1 mL 95% ethanol
colorless liq/ strong, oily-nutty, herbaceous
s—alc, most fixed oils; ins—water/ 174°
1 mL in 1 mL 95% ethanol
almost colorless liq/ metallic, mushroom
s—alc, most fixed oils; ins—prop glycol, water
1 mL in 1 mL 95% ethanol
almost colorless liq/ metallic, mushroom
s—alc, most fixed oils; ss—prop glycol; ins—water
1 mL in 1 mL 95% ethanol
colorless liq/ fresh, piney
s—alc, most fixed oils; ins—water/ 155°
white cryst powder/ vanilla
s—veg oils; ins—water
1 g in 15 mL 95% ethanol
colorless liq/ ethereal
102°
1 mL in 1 mL 95% alc
colorless liq/ ethereal
97°
1 mL in 1 mL 95% alc
H CH3(CH2)5 C C CH2OH H
(Z)-6-Nonen-1-ol Odor, Solubility, Refractive Index revised. FEMA No. 3465 cis-6-Nonen-1-ol
[insert M3465.eps] 142.24/C 9H18O/
3-Octanol Solubility revised. FEMA No. 3581
[insert M3581.eps] 130.23/C 8H18O/
H
H C C
(CH2)4CH2OH
CH3CH2
OH CH3(CH2)4CHCH2CH3
1-Octen-3-yl Acetate Odor, Solubility revised. FEMA No. 3582
[insert M3582.eps] 170.25/C 10H18O2/
CH3(CH2)3CH2CHOOCCH3 CH CH2
1-Octen-3-yl Butyrate Odor, Solubility revised. FEMA No. 3612
[insert M3612.eps] 198.31/C 12H22O2/
CH3(CH2)3CH2CHOOC(CH2)2CH3 CH CH2
␣-Pinene Angular Rotation revised. FEMA No. 2902 2,6,6-Trimethylbicyclo(3.1.1)hept-2-ene; 2-Pinene; l-α-Pinene
[insert M2902.eps] 136.24/C 10H16/
Propenylguaethol Odor, Solubility revised. FEMA No. 2922 1-Ethoxy-2-hydroxy-4propenylbenzene
[insert M2922.eps] 178.23/C 11H14O2/
CH3 H3C CH3
OC2H5 OH
HC CHCH3
Propyl Acetate Odor revised. FEMA No. 2925 n-Propyl Acetate
102.13/C [insert M2925.eps] 5H10O2/
Propyl Alcohol Odor revised. FEMA No. 2928 n-Propanol
60.09/C [insert M2928.eps] 3H8O/
CH3CH2CH2OOCCH3
CH3CH2CH2OH
FCC IV, Supplement 3
Flavor Chemicals / Propyl Alcohol / 87
Requirements I.D. Test4
Assay Min. %5
AV Max.6
Ref. Index7
Sp. Gr.8
IR
96.0% of C9H18O (one major isomer) (M-1a)
1.444–1.448
0.830–0.850
IR
95.0% of C9H18O (M-1a)
1.446–1.452
0.850–0.870
97.0% of C8H18O (M-1a)
1.425–1.429
0.817–0.824
IR
95.0% of C10H18O2 (M-1b)
1.418–1.428
0.865–0.886
IR
95.0% of C12H22O2 (M-1b)
1.423–1.433
0.859–0.880
97.0% of C10H16 (M-1a)
1.464–1.468
0.855–0.860
IR
99.0% of C11H14O2 (M-1a)
IR
97.0% of C5H10O2 (M-1b)
IR
99.0% of C3H8O (M-1b)
Other Requirements9
Angular Rotation—between –20° and –50° (Appendix IIB)
Melting Range—between 85° and 88° (Appendix IIB) Res. on Ignit.—0.1% (Appendix IIC, 2-g sample)
1.0
1.382–1.387
0.880–0.886
1.383–1.388
0.800–0.805
88 / Propyl Propionate / Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Name of Substance Synonyms
Formula Wt/Formula/ Structure
Physical Form/ Odor
Solubility1/ B.P.2
Solubility in Alcohol3
Propyl Propionate Odor revised. FEMA No. 2958 n-Propyl Propionate
[insert M2958.eps] 116.16/C 6H12O2/
colorless to pale yel liq/ fruity
123°
1 mL in 1 mL 95% alc
Terpinen-4-ol Odor revised. FEMA No. 2248 4-Carvomenthenol
[insert M2248.eps] 154.25/C 10H18O/
colorless to pale yel liq/ piney
s—alc/ 88° (6 mm Hg)
(Note: high-purity material may solidify) colorless, viscous liq/ lilac
ss—gly, water/ 217°
1 mL in 2 mL in 60% alc, 8 mL in 50% alc
colorless liq/ sweet, refreshing, herbaceous
s—alc, most fixed oils, min oil, prop glycol; ss—gly; ins—water/ 220°
1 mL in 5 mL 70% alc remains in soln to 10 mL
colorless to slightly yel liq/ sweet, floral, herbaceous, lavender
s—gly; ss—prop glycol; m—alc, chloroform, ether, most fixed oils; ins—water/ 240°
1 mL in 2 mL 80% alc gives clear soln
white or slightly yellowish liq/ oily, citrus
s—alc, most fixed oils; ins—water
1 mL in 1 mL 95% ethanol
gas/ pungent, fishy, ammoniacal
2.9°
colorless to pale yel liq/ melon, green
67° (2.5 mm Hg)
CH3CH2CH2OOCCH2CH3
OH
␣-Terpineol Odor, Assay revised; Note added. FEMA No. 3045 p-Menth-1-en-8-ol
[insert M3045.eps] 154.25/C 10H18O/
OH
Terpinyl Acetate Assay revised. FEMA No. 3047 Menthen-1-yl-8 Acetate
[insert M3047.eps] 196.29/C 12H20O2/
O OC CH3 Terpinyl Propionate Odor, Assay revised. FEMA No. 3053 Menthen-1-yl-8 Propionate
[insert M3053.eps] 210.32/C 13H22O2/
O OC CH2CH3
2-Tridecenal Solubility revised. FEMA No. 3082
196.33/C [insert M3082.eps] 13H24O/
Trimethylamine Ref. Index revised. FEMA No. 3241
[insert M3241.eps] 59.11/C 3H9N/
CH3(CH2)9CH CHCHO
CH3 N H3C
3,5,5-Trimethyl Hexanal Odor revised. FEMA No. 3524
CH3
[insert M3524.eps] 142.24/C 9H18O/ (CH3)3CCH2CH(CH3)CH2CHO
FCC IV, Supplement 3
Flavor Chemicals / 3,5,5-Trimethyl Hexanal / 89
Requirements I.D. Test4
AV Max.6
Ref. Index7
Sp. Gr.8
1.0
1.391–1.396
0.873–0.879
92.0% of C10H18O (M-1b)
1.476–1.480
0.928–0.934
IR
96.0% of C10H18O [sum of α-, (E)-β-, (Z)-β-,γ-, terpinen-4-ol, and terpinen-1-ol isomers] (M-1a)
1.482–1.485
0.930–0.936
IR
97.0% of C12H20O2 [sum of α-, (E)-β-, (Z)-β-, γ-, terpinen4-ol, and terpinen-1ol isomers] (M-1b)
1.464–1.467
0.953–0.962
IR
95.0% of C13H22O2 [sum of α-, (E)-β-, (Z)-β-, γ-, terpinen4-ol, and terpinen-1ol isomers] (M-1b)
1.462–1.468
0.947–0.952
IR
92.0% of C13H24O (M-1a)
1.455–1.460
0.842–0.862
1.419–1.424
0.817–0.823
IR
Assay Min. %5 98.0% of C6H12O2 (M-1b)
1.0
98.0% of C3H9N in a suitable solvent (M-1a)
97.0% (M-1b)
5.0
Other Requirements9
90 / 2,3,5-Trimethylpyrazine/ Flavor Chemicals
FCC IV, Supplement 3
General Information and Description Name of Substance Synonyms
Formula Wt/Formula/ Structure
Physical Form/ Odor
Solubility1/ B.P.2
Solubility in Alcohol3
2,3,5-Trimethylpyrazine Solubility revised. FEMA No. 3244
[insert M3244.eps] 122.17/C7H10N2/
colorless to slightly yel liq/ baked potato, peanut
s—org solvents, water/ 171°
1 mL in 1 mL 95% ethanol
1,3,5-Undecatriene Assay revised. FEMA No. 3795
[insert M3795.eps] 150.26/C 11H18/
clear, colorless to pale yel liq/ oily, waxy, peppery
88° 1 Torr
1 mL in 25 mL 95% alc
(E)-2-Undecenol Solubility in Alcohol added; Ref. Index revised. trans-2-Undecenol
[insert 2Undecen.eps] 170.30/C 11H22O/
white to slightly yel liq/ oily, sweet, floral
ins—water
1 mL in 1 mL 95% ethanol
H 3C
N
CH3
N
CH3
CH3(CH2)7CH CHCH2OH
166.18/C9H10O3/ Veratraldehyde Odor revised. FEMA No. 3109 Methyl Vanillin; Veratryl Aldehyde; 3,4Dimethoxybenzaldehyde
[insert M3109.eps] OCH3 H3CO
Zingerone Odor revised. FEMA No. 3124
[insert M3124.eps] CH2CH2COCH3 HO
white to tan or blue-gray flakes or solid/ sweet, vanilla
1 g in 1 mL 95% alc
CHO
194.23/C11H14O3/
CH3O
yel to yel-brown liq/ spicy
290°
FCC IV, Supplement 3
Flavor Chemicals / Zingerone / 91
Requirements I.D. Test4
Assay Min. %5
AV Max.6
Ref. Index7
Sp. Gr.8
Other Requirements9 Water—0.2% (Appendix IIB, KF; use freshly dist. pyridine as solvent)
IR
98.0% of C7H10N2 (M-1a)
1.503–1.507
0.970–0.980
IR
90.0% of C11H18 [sum of (E),(E)- and (E),(Z)-isomers 60% min] (M1-b)
1.508–1.517
0.787–0.793
IR
92.0% of C11H22O (M-1a)
1.448–1.453
0.840–0.846
IR
95.0% of C9H10O3 (M1-b)
95.0% of C11H14O3 (M-1b)
Solidification Pt.—NLT 40° (Appendix IIB)
1.538–1.545
1.136–1.140
4⁄
Infrared Spectra
Note: The Food Chemicals Codex, Fourth Edition, and its First Supplement, divided the infrared spectra into three categories: Essential Oils, Flavor Chemicals, and Other Substances. The Committee on Food Chemicals Codex has decided to combine all three sections and place the infrared spectra in alphabetical order without reference to category. New samples of all substances whose monographs refer to infrared spectra have been run through the same infrared spectrometer to be the same size and format.
Revision: Insert the following new infrared spectra: Acetaldehyde Diethyl Acetal 2-Acetyl Thiazole Allyl Phenoxy Acetate Allyl Propionate Aspartame–Acesulfame Salt Borneol 2-sec-Butyl Cyclohexanone Butyl 2-Methyl Butyrate
gamma-Cyclodextrin Diphenyl Ether d-Fenchone Fenchyl Alcohol Furfuryl Alcohol 2-Furyl Methyl Ketone Salatrim Sucrose Acetate Isobutyrate
93
94 / Acetaldehyde Diethyl Acetal / Infrared Spectra
FCC IV, Supplement 3
FCC IV, Supplement 3
Infrared Spectra / Allyl Propionate / 95
96 / Aspartame–Acesulfame Salt / Infrared Spectra
FCC IV, Supplement 3
FCC IV, Supplement 3
Infrared Spectra / Butyl 2-Methyl Butyrate / 97
98 / gamma-Cyclodextrin / Infrared Spectra
FCC IV, Supplement 3
FCC IV, Supplement 3
Infrared Spectra / Fenchyl Alcohol / 99
100 / Furfuryl Alcohol / Infrared Spectra
FCC IV, Supplement 3
FCC IV, Supplement 3
Infrared Spectra / Sucrose Acetate Isobutyrate / 101
5⁄
General Tests and Assays
Revised tests and assays (Appendixes I through X in section 5 of the Fourth Edition) are not reprinted in their entirety in his supplement. Refer to the Fourth Edition for unchanged portions; page numbers for the Fourth Edition are provided for this purpose.
APPENDIX III: CHEMICAL TESTS AND DETERMINATIONS
B: LIMIT TESTS
Fluoride Limit Solutions (for a 2-g sample) 50 mg/kg Fluoride Limit Solution (2 mg/kg fluoride standard) Pipet 100 mL of the 10 mg/kg Fluoride Standard into a 500-mL volumetric flask, and dilute to volume with water. 10 mg/kg Fluoride Limit Solution (0.4 mg/kg fluoride standard) Pipet 20 mL of the 10 mg/kg Fluoride Standard into a 500-mL volumetric flask, and dilute to volume with water.
Revision: Method IV reinstated—modified to a pass/fail system, with a 10-mg/kg lower limit.
Note: Store all standard and limit solutions in plastic containers.
FLUORIDE LIMIT TEST, FCC IV, page 758
Sample Preparation Accurately weigh the amount of sample specified in the monograph, transfer it into a 100-mL volumetric flask, and dissolve it in a minimum amount of water. Add 50.0 mL of the Buffer Solution, dilute to volume with water, and mix.
Method IV (Ion-Selective Electrode Method C) Buffer Solution Dissolve 150 g of sodium citrate dihydrate and 10.3 g of disodium EDTA dihydrate in 800 mL of water, adjust the pH to 8.0 with 50% sodium hydroxide solution, and dilute to 1000 mL with water.
Electrode Calibration Pipet 50 mL of the Buffer Solution into a plastic beaker. Place the fluoride ion and reference electrodes (or a combination fluoride electrode) into the plastic beaker and stir. At 5-min intervals, add 100 µL and 1000 µL of the 1000 mg/kg Fluoride Standard and read the potential, in mV, after each addition. The difference between the two readings is the slope of the fluoride electrode and should typically be in the range of 54 to 60 mV at 25°. If the difference in potential is not within this range, check and if necessary, replace, the electrode, instrument, or solutions.
Fluoride Standard Solutions 1000 mg/kg Fluoride Standard Transfer 2.2108 g of sodium fluoride, previously dried at 200° for 4 h, to a 1000-mL volumetric flask and dissolve in and dilute to volume with water. The resulting solution contains 1000 µg of fluoride per mL. 50 mg/kg Fluoride Standard Pipet 50 mL of the 1000 mg/ kg Fluoride Standard into a 1000-mL volumetric flask. Dilute to volume with water. 10 mg/kg Fluoride Standard Pipet 100 mL of the 50 mg/kg Fluoride Standard into a 500-mL volumetric flask. Dilute to volume with water.
Procedure Transfer the entire sample into a plastic beaker. Place the electrode into the beaker, allow the solution to equilibrate for 5 min with stirring, and read the potential, in mV. Remove and rinse the electrode(s) with water. In another beaker, using a pipet, add 50 mL of the Buffer Solution followed by 50 mL of the Fluoride Limit Solution that best reflects the fluoride limit of the sample. Place the electrode in the beaker, equilibrate for 3 min, and read the potential in mV. If the potential of the Fluoride Limit Solution is less than that of the sample, the sample passes the test criterion for maximum acceptable fluoride level limit.
Fluoride Limit Solutions (for a 1-g sample) 50 mg/kg Fluoride Limit Solution (1 mg/kg fluoride standard) Pipet 50 mL of the 10 mg/kg Fluoride Standard into a 500-mL volumetric flask, and dilute to volume with water. 10 mg/kg Fluoride Limit Solution (0.2 mg/kg fluoride standard) Pipet 10 mL of the 10 mg/kg Fluoride Standard into a 500-mL volumetric flask, and dilute to volume with water.
103
104 / Appendix V / General Tests and Assays
FCC IV, Supplement 3
APPENDIX V: ENZYME ASSAYS
This is a new Enzyme Activity Assay:
␣-ACETOLACTATEDECARBOXYLASE ACTIVITY Application and Principle This procedure is used to determine α-acetolactatedecarboxylase (ALDC) activity, expressed as ADU/g. The assay is based on the decarboxylation of α-acetolactate to acetoin by α-Acetolactatedecarboxylase. Acetoin is reacted with a mixture of naphthol and creatine to form a red color for which absorbance is measured at 522 nm. The assay is based on a 20-min decarboxylation of the α-acetolactate substrate at 30° and at pH 6.0. Reagents and Solutions Brij 35 Solution (15%) Dissolve 15.0 g of Brij 35 (Sigma, Catalog No. 430AG-6, or equivalent) in approximately 70 mL of water by heating the solution to 60°. After cooling, transfer the solution to a 100-mL volumetric flask, and dilute to volume with water. Store under refrigeration. The solution is stable for 2 months. MES Buffer (0.05 M) Dissolve 9.76 g of MES [2(N-morpholino)ethanesulfonic acid; Sigma, Catalog No. M8250, or equivalent] in approximately 900 mL of water. Adjust the pH with 1 N sodium hydroxide to 6.00 ± 0.05, and dilute to 1000 mL with water. The buffer is stable for 2 weeks at room temperature. MES Buffer (0.05 M) with Brij 35 (0.05% w/v) and Sodium Chloride (0.6 M) Dissolve 49 g of MES [2(N-morpholino)ethanesulfonic acid; Sigma, Catalog No. M8250, or equivalent] and 175 g of sodium chloride in approximately 4.5 L of water. Add 17 mL of Brij 35 Solution. Adjust the pH with 1 N sodium hydroxide to 6.00 ± 0.05, and dilute to 5 L with water. The buffer is stable for 2 weeks at room temperature. α-Acetolactate Substrate (0.2% v/v) Pipet 100 µL of ethyl2-acetoxy-2-methylacetoacetate (Aldrich, Catalog No. 22,039-6, or equivalent) into a 50-mL volumetric flask. Add 6.0 mL of 0.5 N sodium hydroxide to the volumetric flask, and stir for 20 min. After stirring, add MES Buffer to a volume of approximately 40 mL. Adjust the pH to 6.00 ± 0.05 with 0.5 N hydrochloric acid, and dilute to 50 mL with MES Buffer. Prepare this substrate just before use. Naphthol (1% w/v) and Creatine (0.1% w/v) Color Reagent Dissolve 5.00 g of 1-naphthol (Aldrich, Catalog No. N 199-2, or equivalent) and 0.50 g of creatine (Aldrich, Catalog No. 29,119-6, or equivalent) in 1 N sodium hydroxide in a 500-mL volumetric flask. Prepare the color reagent just before use, and protect it from light. Acetoin Stock Solution Dissolve 0.100 g of acetoin (Aldrich, Catalog No. A1,795-1, or equivalent) in water in a 100-mL volumetric flask. This solution contains 1000 mg of acetoin per L. Acetoin Standard Solutions Dilute Acetoin Stock Solution to prepare the following standards for the standard curve. Use
water as the first standard, concentration 0 mg/L. Pipet 1-, 2-, 4-, 6-, and 8-mL portions of Acetoin Stock Solution into a series of 100-mL volumetric flasks, and dilute each to volume with water. The concentrations of the Acetoin Standard Solutions are 10, 20, 40, 60, and 80 mg/L, respectively. Enzyme Sample Dilute the enzyme samples in MES Buffer with Brij 35 and Sodium Chloride such that the absorbance value of Sample H1 of each sample lies within the absorbance values of the Acetoin Standard curve. Procedure Preheat the Enzyme Sample solutions, the MES Buffer, and the α-Acetolactate Substrate in a 30° water bath for approximately 10 min. Prepare the following solutions for each enzyme sample in the following order: Enzyme Blank B1 Pipet 200 µL of the Enzyme Sample solution into a 10-mL test tube in the 30° water bath. Add 200 µL of MES Buffer, mix, and immediately replace the test tube into the water bath. Sample Value H1 Pipet 200 µL of the Enzyme Sample solution into a 10-mL test tube in the 30° water bath. Add 200 µL of α-Acetolactate Substrate, mix, and immediately replace the test tube into the water bath. Buffer Blank B2 Pipet 200 µL of MES Buffer into a 10-mL test tube in the 30° water bath. Add 200 µL of MES Buffer with Brij 35 and Sodium Chloride, mix, and immediately replace the test tube into the water bath. Buffer Value H2 Pipet 200 µL of MES Buffer with Brij 35 and Sodium Chloride into a 10-mL test tube in the 30° water bath. Add 200 µL of α-Acetolactate Substrate, mix, and immediately replace the test tube into the water bath. Exactly 20 min after mixing the enzyme and buffer (B1), enzyme and substrate (H1), buffer (B2), and buffer and substrate (H2), add 4.6 mL of Naphthol and Creatine Color Reagent to each test tube. Mix, and place the test tubes in a rack at room temperature. Exactly 40 min after adding the Naphthol and Creatine Color Reagent, read the absorbance value, measured at 522 nm, of each sample and blank. Into six separate 10-mL test tubes, pipet 400 µL of each of the five diluted Acetoin Standard Solutions and of water. Add 4.6 mL of Naphthol and Creatine Color Reagent to each test tube, mix, and let the test tubes stand at room temperature. Exactly 40 min after adding the Naphthol and Creatine Color Reagent, read the absorbance value, measured at 522 nm, for each solution. Calculation One α-acetolactatedecarboxylase unit (ADU/g) is the amount of enzyme that produces 1 µmol of acetoin per min by decarboxylation of α-acetolactate under the given reaction conditions. Plot a standard curve from the results of the Acetoin Standard Solutions using the concentration of acetoin, in mg per L, as the abscissa and the absorbance, measured at 522 nm, as the ordinate. Determine the slope, m, of the standard curve. Calculate the enzyme (ALDC) activity of the sample by the formula ADU/g = (Abs × 0.0011351 × F)/(W × m),
FCC IV, Supplement 3
in which Abs = [Abs(H1) – Abs(B1)] – [Abs(H2) – Abs(B2)], F is the sample dilution factor, W is the weight, in grams, of the enzyme sample taken, and 0.0011351 is the number of moles of acetoin in 0.100 gram.
This is a new Enzyme Activity Assay:
AMINOPEPTIDASE (LEUCINE) ACTIVITY Application and Principle This procedure is used to determine leucine aminopeptidase activity in enzyme preparations derived from Lactococcus lactis. The assay is based on the rate of absorbance change over 5 min at 30°; the change in absorbance is due to liberated p-nitroaniline from the hydrolysis of leucine pnitroanilide. Apparatus Spectrophotometer Use a spectrophotometer with temperature control, suitable for measuring absorbancies at 410 nm. Cuvette Use a 10-mm light path, quartz. Thermometer Use a partial immersion thermometer with a suitable range. Vortex Mixer Use a standard, variable-speed mixer. Reagents and Solutions pH 7.0 Phosphate Buffer (100 mM) Dissolve 13.6 g of anhydrous potassium dihydrogen orthophosphate in water, and dilute to 1 L (Solution A). Dissolve 22.8 g of dipotassium hydrogen orthophosphate trihydrate in water, and dilute to 1 L (Solution B). Slowly add approximately 550 mL of Solution B to approximately 400 mL of Solution A until the pH of the buffer stabilizes at 7 ± 0.02. Substrate Solution Dissolve 0.0200 g of leucine p-nitroanilide hydrochloride (Sigma Chemical Co., Catalog No. L2158) in 100 mL of pH 7.0 Phosphate Buffer. p-Nitroaniline Stock Solution Transfer 156.9 mg of pnitroaniline (Aldrich Chemical Co., Catalog No. 18,531-0) to a 1L volumetric flask, and dilute to volume with water. This solution is 1.1136 mM. Caution: p-Nitroaniline is highly toxic. Avoid breathing its dust; avoid contact with skin, eyes, and clothing. Wash the affected area with water; for eyes seek medical attention. Standard p-Nitroaniline Solutions Prepare the following dilutions of p-Nitroaniline Stock Solution: dilute 1 mL of pNitroaniline Stock Solution to 100 mL with pH 7.0 Phosphate Buffer (Solution 1, 0.01136 mM); dilute 9 mL of Solution 1 with 3 mL of pH 7.0 Phosphate Buffer (Solution 2, 0.00852 mM); and dilute 5 mL of Solution 1 with 5 mL of pH 7.0 Phosphate Buffer (Solution 3, 0.00568 mM). Sample Solution Prepare a solution in pH 7.0 Phosphate Buffer that contains between 0.025 and 0.1 unit of aminopeptidase activity per mL.
General Tests and Assays / Appendix V / 105
Procedure Determine the absorbance of each of the three standard p-nitroaniline dilutions (solutions 1, 2, and 3) at 410 nm using pH 7.0 Phosphate Buffer as the blank. Pipet 3 mL of Substrate Solution into a cuvette, insert a thermometer in each to ensure that the temperature of the solution is correct, and equilibrate in the spectrophotometer to 30° ± 0.2°. Add 150 µL of Sample Solution to the equilibrated Substrate Solution. Mix, and start recording the absorbance. Continue recording the absorbance for approximately 5 min; it should increase linearly with time. To determine the rate of change of absorbance, ignore the initial 0.5 min of the assay line, and use a period of at least 4 min to estimate the rate of change. Calculation One aminopeptidase activity unit (AP) is defined as the quantity of aminopeptidase required to liberate 1 µmol/min of leucine from leucine p-nitroanilide under the conditions of the assay at pH 7.0 and 30°. For each of the diluted Standard Solutions—1, 2, and 3— plot absorbance against p-nitroaniline mM concentration. The result is a straight line that passes through the origin. Calculate the millimolar extinction coefficient (ε) of each Standard p-Nitroaniline Solution using the following formula: ε = AN/C, in which AN is the absorbance of the Standard p-Nitroaniline Solution at 410 nm and C is the millimolar concentration of pnitroaniline of that solution. Average the three calculated values; this should result in a value of approximately 8.8. Calculate the activity of each sample taken by the formula: AP/g = (∆A × TCV × 1000)/(ε × SV × C), in which ∆A is the rate of change of absorbance per min; TCV is the total cuvette volume (3.150 mL); SV is the sample volume (0.150 mL); and C is the concentration, in mg/mL, of the sample.
This is a new Enzyme Activity Assay:
LIPASE (MICROBIAL) ACTIVITY FOR MEDIUM- AND LONG-CHAIN FATTY ACIDS Application and Principle This procedure is used to determine the lipase activity in preparations derived from microbial sources. The assay is based on the measurement of the amount of free fatty acids formed from an olive oil emulsion in the presence of sodium taurocholate over a fixed time interval. This assay is particularly used for measuring lipase activity in foods. Reagents and Solutions Acacia (Gum Arabic) Solution Dissolve 110 g of Acacia (gum arabic) (Sigma, Catalog No. G-9752, or equivalent) and 12.5 g of analytical-grade calcium chloride (CaCl2.2H2O) in 800 mL of water in a 1000-mL volumetric flask, and dilute to volume with water. Shake or stir for 30 min at room temperature to
106 / Appendix V / General Tests and Assays
dissolve completely. Centrifuge at 4000 × g for 20 min or filter through a Büchner funnel using Celite as a filter aid. Store the supernatant or filtrate at 4°. Divide into single-use, 24-mL aliquots. The solution is stable for 6 months at –20°. Substrate Emulsion Place 130 mL of olive oil (Sigma, Catalog No. O-1500, or equivalent) and 400 mL of Gum Arabic Solution in a mixer bowl, and cool the mixture to 5° to 10° on ice. Emulsify the mixture with a Waring Blender, or equivalent, operated at high speed for 30 min, keeping the temperature below 30° by repeatedly mixing at high speed for 5 min and turning the blender off for 1 min. Check the quality of the emulsion microscopically: 90% of the droplets should have a diameter equal to or less than 3 µm, and the remaining 10% should not exceed 10 µm. The emulsion is stable for 3 days at 4°. Reference Standard Solution Dissolve an aliquot of Fungi Lipase-International FIP Standard (International Commission on Pharmaceutical Enzymes F.I.P., Center for Standards of the Federation Internationale Pharmaceutique, Harelbekestraat 72, B9000 Gent, Belgium) in a 1% sodium chloride solution and dilute it to obtain a solution of 2.4 to 3.6 FIP microbial lipase units per mL. Prepare this solution fresh. 0.02 N Sodium Hydroxide Solution Prepare daily by diluting 10 mL of analytical-grade 1 N sodium hydroxide to 500 mL with recently boiled water. 0.5% Sodium Taurocholate Solution Dissolve 0.5 g of sodium taurocholate (DIFCO, Catalog No. 0278-15-8) in 100 mL of water. Prepare this solution fresh. Sample Preparation Dissolve an accurately weighed amount of the enzyme preparation in a 1% sodium chloride solution, and dilute to obtain a solution of 2.4 to 3.6 FIP microbial lipase units per mL. Prepare this solution fresh. Procedure (Note: Assay the Fungi Lipase-International FIP Standard as an internal standard each time.) Automatic Titration Use an automatic titration device with a 25 mL ± 0.02 mL buret, a pH meter giving a resolution to 0.01, and a reaction vessel with a capacity of 100 mL. Add 24 mL of Substrate Emulsion, 9 mL of water, and 2 mL of 0.5% Sodium Taurocholate Solution to the reaction vessel. Place the reaction vessel in a water bath preheated to 37° ± 0.5° over a hot plate provided with magnetic stirring, and add a magnet to the reaction vessel. Pre-incubate the reaction vessel at 37° ± 0.5° for 10 to 15 min while stirring at about 300 rpm. Immerse a pH-electrode and the tip of the buret into the solution. If desired, gently blow nitrogen gas onto the solution. Adjust the pH of the solution to 7.0 with 0.02 N Sodium Hydroxide Solution. Set the automatic buret to zero. Add 5.0 mL of the enzyme solution while simultaneously starting a timer. Maintain the pH at 7.0 by automatic titration. After 10.0 min, abruptly (within 30 s) bring the pH to 9.0 by manually adding additional 0.02 N Sodium Hydroxide Solution. Record the volume of 0.02 N Sodium Hydroxide Solution consumed as N1. Run the test with a blank by setting up the titration in the same manner, except after adjusting the pH to 7.0 with 0.02 N Sodium Hydroxide Solution, set the automatic buret to zero, and maintain the pH at 7.0 by automatic titration. After 10.0 min, abruptly (within 30 s) bring the pH to 9.0 as before, and then add 5.0 mL of enzyme solution. Because the enzyme lowers the pH, return the pH to 9.0 by adding 0.02 N Sodium Hydroxide Solution.
FCC IV, Supplement 3
Record the volume of 0.02 N Sodium Hydroxide Solution consumed as N2. Manual Titration Follow the same procedure as with Automatic Titration, but keep the pH at 7.0 with 0.02 N Sodium Hydroxide Solution from a 25-mL buret, demarked in 0.02-mL units. Calculation One unit of enzyme activity (FIP Unit) is defined as that quantity of a standard lipase preparation (Fungi LipaseInternational FIP Standard) that liberates the equivalent of 1 µmol of fatty acid per min from the Substrate Emulsion under the described assay conditions. The specific activity is expressed in international FIP units per mg of the Sample Preparation. The use of an enzyme reference standard of known activity, controlled by the Center for Standards of the Commission, eliminates difficulties from interlaboratory differences in quality of reagents such as the Gum Arabic Solution, olive oil, or Substrate Emulsion or in the set-up of the experiment. The activity (FIP U/ mg) using an enzyme reference standard is calculated by the formula (A × C)/B, in which A is the specific activity, in units/mg, of the test sample (measured); B is the specific activity, in units/mg, of Fungi Lipase-International FIP Standard (measured); and C is the number of FIP units/mg of Fungi Lipase-International FIP Standard as indicated on the container. One mL of the 0.02 N Sodium Hydroxide Solution corresponds with the neutralization of 20 µmol of fatty acids. Five mL of enzyme solution liberates (N1 – N2) mL × 20 µmol of fatty acids over a 10-min time interval. If the enzyme solution contains W mg of enzyme preparation per mL, the specific activity, in units/mg, is calculated as follows: [(N1 – N2) × 20]/(10 × 5 × W), in which (N1 – N2) is the volume, in mL, of the 0.02 N Sodium Hydroxide Solution used for the titration.
This is a new Enzyme Activity Assay:
LYSOZYME ACTIVITY1 Application and Principle The purpose of this procedure is to determine the lysozyme activity in purified lysozyme preparations derived from animal or microbial sources. The assay is based on the rate of decrease in absorbance at 450 nm, attributed to the lysis of Micrococcus lysodeikticus by lysozyme. The decrease in absorbance is measured using a UV/V spectrophotometer equipped to control the sample temperature at 25°.
1Shugar, D. 1952. The measurement of lysozyme activity and the ultra-violet inactivation of lysozyme. Biochimica et Biophysica Acta. 8:302–309.
FCC IV, Supplement 3
Note: Ensure that all glassware and supplies are heat sterilized. The work area should be aseptically clean. Any residual lysozyme contamination will adversely affect the results of the assay. Reagents and Solutions Sodium Phosphate Buffer Solution Dissolve 10.4 g of monobasic sodium phosphate (NaH2PO4.H2O) in 500 mL of sterile, deionized water in a 1000-mL volumetric flask, and dilute to volume. Similarly, dissolve 9.465 g of anhydrous dibasic sodium phosphate (Na2HPO4) in sterile, deionized water, and dilute to 1000 mL. Mix 815 mL of the monobasic sodium phosphate solution with 185 mL of the dibasic sodium phosphate solution. Adjust the pH of the buffer to 6.2; when checking the pH, use an aliquot of the buffer to prevent contamination of the solution. Adjust the pH by adding more monobasic or dibasic sodium phosphate solution as needed. The buffer solution may be stored under refrigeration for up to 1 month. Substrate Solution Add 30 to 40 mg of Micrococcus lysodeikticus (Sigma M-3770, or the equivalent) to 100 mL of Sodium Phosphate Buffer Solution in a 250-mL Erlenmeyer flask, tilt gently to mix, and do not shake. Allow the substrate to incubate at 37° for 30 min before using it. The substrate solution is stable for 2 h at room temperature. Zero a spectrophotometer against air, then measure the absorbance of the substrate solution, which should give a reading of 1.7 ± 0.1 at 450 nm. Note: If the absorbance is significantly lower than 1.7, do not adjust the concentration. Run the analysis, and check the rate of the reaction. The rate of the decrease in absorbance should range between 0.03 and 0.06 unit per min. Standard Preparation Use a commercial reference standard lysozyme of a specified strength from an animal or microbial source in accordance with the origin of the preparation being measured. Measure 50 mg of the reference standard lysozyme into a 50-mL volumetric flask, and dissolve, with stirring, in approximately 25 mL of Sodium Phosphate Buffer Solution. Dilute to volume with Sodium Phosphate Buffer Solution, and mix thoroughly. If desired, freeze aliquots of this Standard Preparation for subsequent assays. Quantitatively transfer 3 mL of the Standard Preparation to a 100-mL volumetric flask, and dilute to volume with Sodium Phosphate Buffer Solution.
General Tests and Assays / Appendix V / 107
Sample Preparation Measure 50 mg of sample into a 50mL volumetric flask. Dissolve the sample, with stirring, in approximately 25 mL of Sodium Phosphate Buffer Solution. Dilute to volume with Sodium Phosphate Buffer Solution, and mix the solution thoroughly. Quantitatively transfer 3 mL of the solution to a 100-mL volumetric flask, and dilute to volume with Sodium Phosphate Buffer Solution. Procedure Conduct the test in a spectrophotometer equipped to maintain a temperature of 25° in the cell compartment. Perform the test in triplicate for the Standard Preparation and for the Sample Preparation. Place a 1-cm cell into the spectrophotometer, and adjust the absorbance to zero. Pipet 2.9 mL of Substrate Solution into the cell; the initial absorbance of the solution should be 1.7 ± 0.1 at 450 nm (see NOTE above). Pipet 0.1 mL of the Standard Preparation into the substrate, and mix well. Record the decrease in absorbance over 3 min, recording the absorbance value approximately every 15 s. The rate of the decrease in absorbance should be linear, and range between 0.03 and 0.06 per min. Repeat the procedure with the Sample Preparation. Calculation One lysozyme unit is defined as the amount of lysozyme that causes a decrease in absorbance of 0.001 per min at 450 nm, 25°, and pH 6.2, using a suspension of Micrococcus lysodeikticus as the substrate. The assay stabilizes over the first min; disregard the first min of readings in the calculation. Determine the average absorbance change per min using only the linear portion of the curve where the rate of change is constant, usually the final 2 min. Calculate the number of lysozyme units per mg by the formula lysozyme units = (A1 – A2)/(T × W × 0.001), in which A1 is the initial absorbance reading in the straight-line portion of the curve; A2 is the final absorbance reading in the straight-line portion of the curve; T is the elapsed time, in min, between the initial and final absorbance readings; W is the weight, in mg, of the lysozyme in the volume of Sample Preparation used in the Assay; and 0.001 is the decrease in absorbance caused by one unit of lysozyme per min.
108 / Appendix VII / General Tests and Assays
FCC IV, Supplement 3
APPENDIX VII: FATS AND RELATED SUBSTANCES
Revision: A second Peroxide Value test has been added.
PEROXIDE VALUE, FCC IV, SECOND SUPPLEMENT, page 43
Unless otherwise indicated in the monograph, use Method I: Acetic Acid–Isooctane Method. The peroxide value is defined as the number of milliequivalents of peroxide per 1000 g of sample that oxidizes potassium iodide under the given test conditions. Method I: Acetic Acid–Isooctane Method Method Cd 8b-90)
(Based on AOCS
Solutions Acetic Acid–Isooctane Solution Mix 3 volumes of glacial acetic acid with 2 volumes of isooctane. Note: Use a fume hood at all times, and avoid inhalation, ingestion, and skin contact. Saturated Potassium Iodide Solution Dissolve an excess of potassium iodide in recently boiled water. Prepare fresh daily, and make certain the solution remains saturated during use. Starch Indicator Solution Make a paste with 1 g of starch and a small amount of cold water, and add it, while stirring, to 200 mL of boiling water. Remove from heat within a few s, and cool. If desired, add salicylic acid (1.25 g/L) as a preservative. The solution may be kept refrigerated at 4° to 10° for not more than 3 weeks. Test the solution for sensitivity before use by placing 5 mL of the solution in 100 mL of water and adding 0.05 mL of 0.1 N potassium iodide solution. The deep blue color produced must be discharged by 0.05 mL of 0.1 N sodium thiosulfate. If the solution fails the test, prepare a fresh starch solution. Procedure Accurately weigh 5.00 g ± 0.05 g of sample, transfer into a 250-mL Erlenmeyer flask with a glass stopper, and add 50 mL of Acetic Acid–Isooctane Solution. Swirl to dissolve the sample, and add 0.5 mL of Saturated Potassium Iodide Solution.
Allow the sample solution to stand, agitating it occasionally, for exactly 1 min, and immediately add 30 mL of water. Titrate with 0.1 N sodium thiosulfate solution, adding the solution gradually while constantly agitating until the yellow iodine color has almost disappeared. Add 0.5 mL of a 10% sodium lauryl sulfate (SDS) solution, and then add approximately 0.5 mL of Starch Indicator Solution. Continue the titration while constantly agitating, especially near the endpoint to liberate all of the iodine from the solvent layer. Add 0.1 N thiosulfate solution dropwise until the blue color just disappears. If the titration is less than 0.5 mL using 0.1 N sodium thiosulfate, repeat the determination using 0.01 N sodium thiosulfate. Conduct a blank determination, and make any necessary correction. Calculate the peroxide value by the formula [(S – B) × N × 1000]/W, in which S is the volume, in mL, of 0.1 N sodium thiosulfate consumed by the sample; B is the volume, in mL, of 0.1 N sodium thiosulfate consumed by the blank; N is the normality of the sodium thiosulfate solution; and W is the weight, in g, of the sample taken. Method II (Alternatively, follow AOCS Method Cd 8-53) Note: To make the solutions referenced below, please see the Fourth Edition, pages 859 (0.1 N sodium thiosulfate solution— diluted 1:1 v/v) and 855 (starch TS). Accurately weigh about 10 g of the sample, add 30 mL of a 3:2 mixture of glacial acetic acid:chloroform, and mix. Add 1 mL of a saturated solution of potassium iodide, and mix for 1 min. Add 100 mL of water, begin titrating with 0.05 N sodium thiosulfate, adding starch TS as the endpoint is approached, and continue the titration until the blue starch color has just disappeared. Perform a blank determination (see General Provisions), and make any necessary correction. Calculate the peroxide value, as milliequivalents of peroxide per kilogram of sample, by the formula S × N × 1000/W, in which S is the net volume, in mL, of sodium thiosulfate solution required for the sample; N is the exact normality of the sodium thiosulfate solution; and W is the weight, in g, of the sample taken.
FCC IV, Supplement 3
General Tests and Assays / Appendix VIII / 109
APPENDIX VIII: OLEORESINS
Revision: Product source provided.
CURCUMIN CONTENT, FCC IV, page 829 Standard Preparation Transfer about 250 mg of pure curcumin (Sigma Chemical), accurately weighed, into a 100-mL volumetric flask, and record the weight as W, in mg. Dissolve in acetone, dilute to volume with acetone, and mix. Pipet a 1-mL portion of this solution into a second 100-mL volumetric flask, dilute to volume with acetone, and mix. Finally, pipet a 5-mL portion of the last solution into a 50-mL volumetric flask, dilute to volume with acetone, and mix. Sample Preparation Transfer an accurately weighed amount of the sample, equivalent to about 250 mg of curcumin, into a 100mL volumetric flask, and record the weight as w, in mg. Dissolve in acetone, dilute to volume with acetone, and mix. Pipet a 1-mL
portion of this solution into a second 100-mL volumetric flask, dilute to volume with acetone, and mix. Finally, pipet a 5-mL portion of the last solution into a 50-mL volumetric flask, dilute to volume with acetone, and mix. Procedure Determine the absorbance of each solution in 1-cm cells at the wavelength of maximum absorption at about 421 nm with a suitable spectrophotometer, using acetone as the blank. Calculate the percentage of curcumin in the sample by the formula 100 × (W/w) × (AU/AS), in which AU is the absorbance of the Sample Preparation, and AS is the absorbance of the Standard Preparation. Note: The absorbance readings should be made as soon as possible after the solutions are prepared to avoid color loss.
110 / Solutions and Indicators / General Tests and Assays
SOLUTIONS AND INDICATORS, FCC IV, page 848 This is a new Test Solution: Acetic Acid TS, Strong (5 N) A solution containing 30% v/v of CH3COOH. Prepare by diluting 300.0 mL of glacial acetic acid with sufficient water to make 1000 mL.
This is a new Test Solution: Nickel Standard Solution TS (10 mg/kg) Prepare a 0.400% w/ v solution of analytical reagent-grade nickel chloride (NiCl2. 6H2O) with water. Pipet 1.0 mL of the solution into a 100-mL volumetric flask, and dilute to volume with water.
Revision: Form of quinoline revised. Quimociac TS Dissolve 70 g of sodium molybdate (Na2MoO4. 2H2O) in 150 mL of water (Solution A). Dissolve 60 g of citric acid in a mixture of 85 mL of nitric acid and 150 mL of water, and cool (Solution B). Gradually add Solution A to Solution B, with stirring, to produce Solution C. Dissolve 5.0 mL of natural or synthetic quinoline in a mixture of 35 mL of nitric acid and 100 mL of water (Solution D). Gradually add Solution D to Solution C, mix well, and allow to stand overnight. Filter the mixture, add 280 mL of acetone to the filtrate, dilute to 1000 mL with water, and mix. Store in a polyethylene bottle.
FCC IV, Supplement 3
Caution: This reagent contains acetone. Do not use it near an open flame. Operations involving heating or boiling should be conducted in a well-ventilated hood.
Revision: Use of barium hydroxide removed. Sodium Hydroxide, 1 N (40.00 g NaOH per 1000 mL) Dissolve about 40 g of sodium hydroxide (NaOH) in about 1000 mL of carbon dioxide-free water. Shake the mixture thoroughly, and allow it to stand overnight in a stoppered bottle. Standardize the clear liquid as follows: Transfer about 5 g of primary standard potassium biphthalate [KHC6H4(COO)2], previously dried at 105° for 2 h and accurately weighed, to a flask, and dissolve it in 75 mL of carbon dioxide-free water. If the potassium biphthalate is in the form of large crystals, crush it before drying. To the flask add 2 drops of Phenolphthalein TS, and titrate with the sodium hydroxide solution to a permanent pink color. Calculate the normality. Each 204.2 mg of potassium biphthalate is equivalent to 1 mL of 1 N Sodium Hydroxide. Note: Solutions of alkali hydroxides absorb carbon dioxide when exposed to air. Therefore, store them in bottles with well-fitted, suitable stoppers provided with a tube filled with a mixture of sodium hydroxide and lime so that air entering the container must pass through this tube, which will absorb the carbon dioxide. Frequently restandardize standard solutions of sodium hydroxide.
Index Titles of monographs in Section 2, those of flavor chemicals in Section 3, and those of tests in the Appendixes are shown in boldface type. An asterisk indicates a new item for this Third Supplement to the Fourth Edition of the Food Chemicals Codex. Other titles refer to revised items or to secondary names of the substances. Revised test methods listed in this Supplement may not be given in their entirety; only the corrected sections are generally shown. For this reason, a bold page number after a test name indicates the entire test method’s location in the Fourth Edition, while the standard page number indicates its location in this Third Supplement.
A Acetal, 64 *Acetaldehyde Diethyl Acetal, 64, 94 *Acetic Acid TS, Strong (Solutions and Indicators), 110 Acetoacetic Ester, 72 Acetoin, 64 α-Acetolactatedecarboxylase (Bacillus subtilis containing a Bacillus brevis gene), 19 *α-Acetolactatedecarboxylase Activity (Appendix V), 104 Acetyl Methyl Carbinol, 64 2-Acetylpyrrole, 64 *2-Acetyl Thiazole, 64, 94 *Acidified Sodium Chlorite Solutions, 3 Alcohol C-6, 76 ALDC Activity, 110 Aldehyde C-7, 76 Allura Red AC, 27 Allyl Isothiocyanate, 64 *Allyl Phenoxy Acetate, 64, 95 *Allyl Propionate, 66, 95 L-2-Amino-5-guanidinovaleric Acid, 5 L-2-Amino-3-hydroxybutyric Acid, 60 DL-2-Amino-3-hydroxypropanoic Acid, 50 L-2-Amino-3-hydroxypropanoic Acid, 50 L-2-Amino-3-methylbutyric Acid, 62 DL-2-Amino-3-methylvaleric Acid, 30 DL-2-Amino-4-methylvaleric Acid, 32 L-2-Amino-3-methylvaleric Acid, 31 *Aminopeptidase (Leucine) Activity (Appendix V), 105 Aminopeptidase, Leucine (Aspergillus niger var., Aspergillus oryzae var., and other microbial species), 19
DL-Aminosuccinic Acid,
7 7 Ammonium Phosphate, Dibasic, 4 Ammonium Phosphate, Monobasic, 4 1-Amyl Alcohol, 66 Amylase, 18 Amyl Butyrate, 66 Amyl Formate, 66 Amyl Salicylate, 78 Anhydrous Lanolin, 31 Animal Lipase, 18 APM–Ace, 5 L-Arginine, 5 *Aspartame–Acesulfame Salt, 5, 96 dl-Aspartic Acid, 7 L-Aspartic Acid, 7 L-α-aspartyl-2-methyl ester compound with 6 methyl-1,2,3-oxathiazin-4(3H)one 2,2-dioxide (1:1), 5 L-Aminosuccinic Acid,
B Beta-1,3-glucan, 15 Bleidner Apparatus, 17 *Borneol, 66, 96 Bovine Rennet, 18 Brilliant Blue FCF, 24 Bromelain, 18 *2-sec-Butyl Cyclohexanone, 66, 97 *Butyl 2-Methyl Butyrate, 66, 97 Butyric Acid, 66
C Calf Rennet, 18 Canola Oil, 8
111
Carbohydrase (Aspergillus niger var., including Aspergillus aculeatus), 19 Carbohydrase (Aspergillus oryzae var.), 19 Carbohydrase (Bacillus acidopullulyticus), 19 Carbohydrase (Bacillus stearothermophilus), 19 Carbohydrase (Bacillus subtilis containing a Bacillus megaterium αamylase gene), 19 Carbohydrase (Bacillus subtilis containing a Bacillus stearothermophilus α-amylase gene), 19 Carbohydrase (Candida pseudotropicalis), 19 Carbohydrase (Kluyveromyces marxianus var. lactis), 19 Carbohydrase (Mortierella vinaceae var. raffinoseutilizer), 19 Carbohydrase (Rhizopus niveus), 19 Carbohydrase (Rhizopus oryzae var.), 19 Carbohydrase (Saccharomyces species), 19 Carbohydrase (Trichoderma longibrachiatum var.; formerly reesei), 20 Carbohydrase and Protease, Mixed (Bacillus licheniformis var.), 20 Carbohydrase and Protease, Mixed (Bacillus subtilis var. including Bacillus amyloliquefaciens), 20 [2-Carboxy-β-(N-(b-methoxycarbonyl-2phenyl)ethylcarbamoyl)]ethanaminium 6-Methyl-4-oxo-1,2,3-oxathiazin-3ide-2,2-dioxide, 5
112 / Index
Carmine, 10 Carminic Acid, 10 4-Carvomenthenol, 88 Catalase (Aspergillus niger var.), 20 Catalase (bovine liver), 18 Catalase (Micrococcus lysodeikticus), 20 gamma-CD, 16 Cellulose Gum, 11 Chymosin (Aspergillus niger var. awamori, Escherichia coli K-12, and Kluyveromyces marxianus, each microorganism containing a calf prochymosin gene), 20 Chymotrypsin, 18 Cinnamic Acid, 66 Citric Acid, 12 CMC, 11 Cocoa Butter Substitute, 13 Cornmint Oil, Partially Dementholized, 34 Curcumin Content (Appendix VIII), 109 *Curdlan, 15 γ-Cyclodextrin, 16 *gamma-Cyclodextrin, 16, 98 Cyclohexyl Acetate, 68 Cyclomaltooctaose, 16 Cyclooctaamylose, 16 p-Cymene, 68
D (E),(E)-2,4-Decadienal, 68 trans,trans-2,4-Decadienal, 68 cis-4-Decenal, 68 (E)-2-Decenal, 68 trans-2-Decenal, 68 (Z)-4-Decenal, 68 Diammonium Phosphate, 4 Dibasic Ammonium Phosphate, 4 Dibasic Sodium Phosphate, 53 1,2-Di-[(1'-ethoxy)ethoxy]propane, 68 Dihydrocarveol, 68 d-Dihydrocarvone, 68 3,4-Dimethoxybenzaldehyde, 90 Dimethyl Benzyl Carbinyl Butyrate, 70 Dimethylketol, 64 α,α-Dimethylphenethyl Butyrate, 70 2,3-Dimethylpyrazine, 70 2,5-Dimethylpyrrole, 70 Dimethyl Succinate, 70 Dimethyl Sulfide, 70 *Diphenyl Ether, 70, 98 Diphenyl Oxide, 70 Disodium Dihydrogen Pyrophosphate, 52 Disodium Monohydrogen Phosphate, 53
FCC IV, Supplement 3
Disodium Phosphate, 53 Disodium Pyrophosphate, 52 δ-Dodecalactone, 70 (E)-2-Dodecen-1-al, 70 trans-2-Dodecen-1-al, 70
E Enocianina, 29 Enzyme Activity (Appendix V), 104 *α-Acetolactatedecarboxylase Activity, 104 *Aminopeptidase (Leucine) Activity, 105 *Lipase (Microbial) Activity for Medium- and Long-Chain Fatty Acids, 105 *Lysozyme Activity, 106 Enzyme Preparations, 17 Animal-Derived Preparations, 18 Catalase (bovine liver), 18 Chymotrypsin, 18 Lipase, Animal, 18 *Lysozyme, 18 Pancreatin, 18 Pepsin, 18 Phospholipase A2, 18 Rennet, Bovine, 18 Rennet, Calf, 18 Trypsin, 18 Plant-Derived Preparations, 18 Amylase, 18 Bromelain, 18 Ficin, 18 Malt, 18 Papain, 18 Microbially Derived Preparations, 19 *α-Acetolactatedecarboxylase (Bacillus subtilis containing a Bacillus brevis gene), 19 *Aminopeptidase, Leucine (Aspergillus niger var., Aspergillus oryzae var., and other microbial species), 19 Carbohydrase (Aspergillus niger var., including Aspergillus aculeatus), 19 Carbohydrase (Aspergillus oryzae var.), 19 Carbohydrase (Bacillus acidopullulyticus), 19 Carbohydrase (Bacillus stearothermophilus), 19 Carbohydrase (Bacillus subtilis containing a Bacillus megaterium α-amylase gene), 19 Carbohydrase (Bacillus subtilis containing a Bacillus
stearothermophilus α-amylase gene), 19 Carbohydrase (Candida pseudotropicalis), 19 Carbohydrase (Kluyveromyces marxianus var. lactis), 19 Carbohydrase (Mortierella vinaceae var. raffinoseutilizer), 19 Carbohydrase (Rhizopus niveus), 19 Carbohydrase (Rhizopus oryzae var.), 19 Carbohydrase (Saccharomyces species), 19 Carbohydrase (Trichoderma longibrachiatum var.; formerly reesei), 20 Carbohydrase and Protease, Mixed (Bacillus licheniformis var.), 20 Carbohydrase and Protease, Mixed (Bacillus subtilis var. including Bacillus amyloliquefaciens), 20 Catalase (Aspergillus niger var.), 20 Catalase (Micrococcus lysodeikticus), 20 Chymosin (Aspergillus niger var. awamori, Escherichia coli K-12, and Kluyveromyces marxianus, each microorganism containing a calf prochymosin gene), 20 Glucose Isomerase (Actinoplanes missouriensis, Bacillus coagulans, Streptomyces olivaceus, Streptomyces olivochromogenes, Microbacteruim arborescens, Streptomyces rubiginosus var., or Streptomyces murinus), 20 Glucose Oxidase (Aspergillus niger var.), 20 Lipase (Aspergillus niger var.), 20 Lipase (Aspergillus oryzae var.), 20 Lipase (Candida rugosa; formerly Candida cylindracea), 20 Lipase (Rhizomucor (Mucor) miehei), 20 Phytase (Aspergillus niger var.), 20 Protease (Aspergillus niger var.), 20 Protease (Aspergillus oryzae var.), 21 Rennet, Microbial (nonpathogenic strain of Bacillus cereus), 21 Rennet, Microbial (Endothia parasitica), 21 Rennet, Microbial (Rhizomucor (Mucor) sp.), 21 Erythrosine, 26 Ethone, 72
FCC IV, Supplement 3
6-Ethoxy-1,2-dihydro-2,2,4trimethylquinoline, 23 1-Ethoxy-2-hydroxy-4-propenylbenzene, 86 Ethoxyquin, 23 Ethyl Acetoacetate, 72 Ethyl Benzoyl Acetate, 72 Ethyl-(E)-2-butenoate, 72 Ethyl-trans-2-butenoate, 72 Ethyl Crotonate, 72 Ethylene Brassylate, 72 2-Ethyl Hexanol, 72 2-Ethyl-1-hexanol, 72 Ethyl 2-Hydroxypropionate, 72 Ethyl Lactate, 72 Ethyl Levulinate, 72 Ethyl 2-Methylbutyrate, 72 Ethyl 2-Methylpentanoate, 74 Ethyl 3-Methylthiopropionate, 74 Ethyl 3-Oxybutanoate, 72 Ethyl n-Pentanoate, 74 Ethyl Salicylate, 74 Ethyl 10-Undecenoate, 74 Ethyl Valerate, 74
F Farnesol, 74 Fast Green FCF, 25 FD&C Blue No. 1, 24 FD&C Blue No. 2, 24 FD&C Green No. 3, 25 FD&C Red No. 3, 26 FD&C Red No. 40, 27 FD&C Yellow No. 5, 28 FD&C Yellow No. 6, 29 *d-Fenchone, 74, 99 *Fenchyl Alcohol, 74, 99 Ficin, 18 Flavor Chemicals, 63 Acetaldehyde Diethyl Acetal, 64 Acetoin, 64 2-Acetylpyrrole, 64 2-Acetyl Thiazole, 64 Allyl Isothiocyanate, 64 Allyl Phenoxy Acetate, 64 Allyl Propionate, 66 1-Amyl Alcohol, 66 Amyl Butyrate, 66 Amyl Formate, 66 Borneol, 66 2-sec-Butyl Cyclohexanone, 66 Butyl 2-Methyl Butyrate, 66 Butyric Acid, 66 Cinnamic Acid, 66 Cyclohexyl Acetate, 68 p-Cymene, 68 (E),(E)-2,4-Decadienal, 68
Index / 113
(E)-2-Decenal, 68 (Z)-4-Decenal, 68 1,2-Di-[(1′-ethoxy)ethoxy]propane, 68 Dihydrocarveol, 68 d-Dihydrocarvone, 68 Dimethyl Benzyl Carbinyl Butyrate, 70 2,3-Dimethylpyrazine, 70 2,5-Dimethylpyrrole, 70 Dimethyl Succinate, 70 Dimethyl Sulfide, 70 Diphenyl Ether, 70 δ-Dodecalactone, 70 (E)-2-Doceden-1-al, 70 Ethone, 72 Ethyl Acetoacetate, 72 Ethyl Benzoyl Acetate, 72 Ethyl-(E)-2-butenoate, 72 Ethylene Brassylate, 72 2-Ethyl Hexanol, 72 Ethyl Lactate, 72 Ethyl Levulinate, 72 Ethyl 2-Methylbutyrate, 72 Ethyl 2-Methylpentanoate, 74 Ethyl 3-Methylthiopropionate, 74 Ethyl Salicylate, 74 Ethyl 10-Undecenoate, 74 Ethyl Valerate, 74 Farnesol, 74 d-Fenchone, 74 Fenchyl Alcohol, 74 Furfuryl Alcohol, 74 2-Furyl Methyl Ketone, 74 Fusel Oil, Refined, 76 (E),(E)-2,4-Heptadienal, 76 Heptanal, 76 2-Heptanone, 76 (Z)-4-Hepten-1-al, 76 (E)-2-Hexen-1-al, 76 (Z)-3-Hexenyl Isovalerate, 76 (Z)-3-Hexenyl 2-Methylbutyrate, 76 Hexyl Alcohol, 76 Hexyl Isovalerate, 78 Hexyl 2-Methylbutyrate, 78 Isoamyl Alcohol, 78 Isoamyl Benzoate, 78 Isoamyl Butyrate, 78 Isoamyl Phenyl Acetate, 78 Isoamyl Salicylate, 78 Isobutyl Cinnamate, 78 Isobutyraldehyde, 78 Isopropyl Acetate, 80 Levulinic Acid, 80 l-Limonene, 80 Menthol, 80 l-Menthone, 80 dl-Menthyl Acetate, 80 l-Menthyl Acetate, 80
2-Methoxy-3(5)-methylpyrazine, 82 2-Methyl Butanal, 82 3-Methyl Butanal, 82 2-Methylbutyl Acetate, 82 2-Methylbutyl Isovalerate, 82 Methyl Butyrate, 82 2-Methylbutyric Acid, 82 Methyl Ionones, 82 Methyl Isobutyrate, 82 Methyl-3-methylthiopropionate, 82 4-Methyl-2-pentanone, 84 Methyl Propyl 3-Methyl Butyrate, 84 4-Methyl-5-thiazole Ethanol, 84 Nerolidol, 84 (E),(E)-2,4-Nonadienal, 84 (E),(Z)-2,6-Nonadienal, 84 (E),(Z)-2,6-Nonadienol, 84 Nonanoic Acid, 84 (E)-2-Nonenal, 84 (E)-2-Nonen-1-ol, 86 (Z)-6-Nonen-1-ol, 86 3-Octanol, 86 1-Octen-3-yl Acetate, 86 1-Octen-3-yl Butyrate, 86 α-Pinene, 86 Propenylguaethol, 86 Propyl Acetate, 86 Propyl Alcohol, 86 Propyl Propionate, 88 Terpinen-4-ol, 88 α-Terpineol, 88 Terpinyl Acetate, 88 Terpinyl Propionate, 88 2-Tridecenal, 88 Trimethylamine, 88 3,5,5-Trimethyl Hexanal, 88 2,3,5-Trimethylpyrazine, 90 1,3,5-Undecatriene, 90 (E)-2-Undecenol, 90 Veratraldehyde, 90 Zingerone, 90 Fluoride Limit Test (Method IV), 103 Freskomenthe, 66 Fully Hydrogenated Rapeseed Oil, 44 *Furfuryl Alcohol, 74, 100 *2-Furyl Methyl Ketone, 74, 100 Fusel Oil, Refined, 76
G Glassy Sodium Polyphosphates, 55 α-D-Glucopyranosyl-1,4-D-glucitol, 33 Glucose Isomerase (Actinoplanes missouriensis, Bacillus coagulans, Streptomyces olivaceus, Streptomyces olivochromogenes, Microbacteruim arborescens, Streptomyces
114 / Index
rubiginosus var., or Streptomyces murinus), 20 Glucose Oxidase (Aspergillus niger var.), 20 Glycerol Esters of Condensed Castor Oil Fatty Acids, 38 Glyceryl Triacetate, 61 Graham’s Salt, 55 Grape Skin Extract, 29
H Heavy Metals Limits Policy, 1 (E),(E)-2,4-Heptadienal, 76 trans,trans-2,4-Heptadienal, 76 Heptaldehyde, 76 Heptanal, 76 2-Heptanone, 76 cis-4-Hepten-1-al, 76 (Z)-4-Hepten-1-al, 76 2,4-Hexadienoic Acid, 59 2,4-Hexadienoic Acid, Potassium Salt, 42 1-Hexanol, 76 (E)-2-Hexen-1-al, 76 trans-2-Hexen-1-al, 76 cis-3-Hexenyl Isovalerate, 76 (Z)-3-Hexenyl Isovalerate, 76 cis-3-Hexenyl 2-Methylbutyrate, 76 (Z)-3-Hexenyl 2-Methylbutyrate, 76 Hexyl Alcohol, 76 Hexyl Isovalerate, 78 Hexyl 2-Methylbutyrate, 78 Hydrogenated Maltose, 33 3-Hydroxy-2-butanone, 64
I IMP, 52 Indigo Carmine, 24 Indigotine, 24 Infrared Spectra, 93 Acetaldehyde Diethyl Acetal, 94 2-Acetyl Thiazole, 94 Allyl Phenoxy Acetate, 95 Allyl Propionate, 95 Aspartame–Acesulfame Salt, 96 Borneol, 96 2-sec-Butyl Cyclohexanone, 97 Butyl 2-Methyl Butyrate, 97 gamma-Cyclodextrin, 98 Diphenyl Ether, 98 d-Fenchone, 99 Fenchyl Alcohol, 99 Furfuryl Alcohol, 100 2-Furyl Methyl Ketone, 100 Salatrim, 101 Sucrose Acetate Isobutyrate, 101
FCC IV, Supplement 3
Insoluble Sodium Metaphosphate, 52 Insoluble Sodium Polyphosphate, 52 Isoamyl Alcohol, 78 Isoamyl Benzoate, 78 Isoamyl Butyrate, 78 Isoamyl Phenyl Acetate, 78 Isoamyl Salicylate, 78 Isobutyl Cinnamate, 78 Isobutyl Isovalerate, 84 Isobutyraldehyde, 78 DL-Isoleucine, 30 L-Isoleucine, 31 Isopropyl Acetate, 80
L Lanolin, Anhydrous, 31 LEAR, 8 Lemongrass Oil, 32 DL-Leucine, 32 Leucine Aminopeptidase, 19 Levulinic Acid, 80 l-Limonene, 80 Lipase, Animal, 18 Lipase (Aspergillus niger var.), 20 Lipase (Aspergillus oryzae var.), 20 Lipase (Candida rugosa; formerly Candida cylindracea), 20 *Lipase (Microbial) Activity for Medium- and Long-Chain Fatty Acids (Appendix V), 105 Lipase (Rhizomucor (Mucor) miehei), 20 Lovage Oil, 33 Low Erucic Acid Rapeseed Oil, 8 Low Linolenic Acid Flaxseed Oil (Unhydrogenated), 58 Low Linolenic Acid Linseed Oil, 58 Lysozyme, 18 *Lysozyme Activity (Appendix V), 106
dl-Menthyl Acetate, 80 l-Menthyl Acetate, 80 2-Methoxy-3(5)-methylpyrazine, 82 1-(p-Methoxyphenyl)-1-penten-3-one, 72 Methyl Amyl Ketone, 76 2-Methyl Butanal, 82 3-Methyl Butanal, 82 2-Methylbutyl Acetate, 82 2-Methylbutyl Isovalerate, 82 2-Methylbutyl-3-methylbutanoate, 82 Methyl Butyrate, 82 2-Methylbutyric Acid, 82 Methyl Ionones, 82 Methyl Isobutyl Ketone, 84 Methyl Isobutyrate, 82 d-2-Methyl-5-(1-methylethenyl)cyclohexanone, 68 Methyl-3-methylthiopropionate, 82 4-Methyl-2-pentanone, 84 2-Methyl Propyl 3-Methyl Butyrate, 84 Methyl 2-Pyrrolyl Ketone, 64 Methyl Sulfide, 70 4-Methyl-5-thiazole Ethanol, 84 Methyl Vanillin, 90 Microbial Rennet (nonpathogenic strain of Bacillus cereus), 21 Microbial Rennet (Endothia parasitica), 21 Microbial Rennet (Rhizomucor (Mucor) sp.), 21 Mixed Carbohydrase and Protease, 20 Modified Cellulose, 11 Monoammonium Phosphate, 4 Monobasic Potassium Phosphate, 40 Monobasic Sodium Phosphate, 54 Monopotassium Phosphate, 40 Monosodium Dihydrogen Phosphate, 54 Monosodium Phosphate, 54
M Maddrell’s Salt, 52 Malt, 18 Maltitol, 33 D-Maltitol, 33 Mentha Arvensis Oil, Partially Dementholized, 34 l-p-Mentha-1,8-diene, 80 3-p-Menthanol, 80 l-p-Menthan-3-one, 80 dl-p-Menthan-3-yl Acetate, 80 l-p-Menthan-3-yl Acetate, 80 p-Menth-1-en-8-ol, 88 Menthen-1-yl-8 Acetate, 88 Menthen-1-yl-8 Propionate, 88 Menthol, 80 l-Menthone, 80
N Nerolidol, 84 *Nickel Standard Solution TS (Solutions and Indicators), 110 (E),(E)-2,4-Nonadienal, 84 (E),(Z)-2,6-Nonadienal, 84 trans,cis-2,6-Nonadienal, 84 trans,trans-2,4-Nonadienal, 84 (E),(Z)-2,6-Nonadienol, 84 trans,cis-2,6-Nonadienol, 84 Nonanoic Acid, 84 (E)-2-Nonenal, 84 trans-2-Nonenal, 84 cis-6-Nonen-1-ol, 86 (E)-2-Nonen-1-ol, 86 trans-2-Nonen-1-ol, 86
FCC IV, Supplement 3
(Z)-6-Nonen-1-ol, 86
O 3-Octanol, 86 1-Octen-3-yl Acetate, 86 1-Octen-3-yl Butyrate, 86
P Pancreatin, 18 Papain, 18 Partially Dementholized Mentha Arvensis Oil, 34 Pectins, 35 1-Pentanol, 66 Pentapotassium Triphosphate, 43 Pentasodium Triphosphate, 57 1-Pentyl Butyrate, 66 1-Pentyl Formate, 66 Pepsin, 18 Peroxide Value (Appendix VII), 108 L-Phenylalanine, 5 3-Phenylpropenoic Acid, 66 Phospholipase A2, 18 Phytase (Aspergillus niger var.), 20 2-Pinene, 86 ␣-Pinene, 86 l-α-Pinene, 86 Polyglycerol Esters of Interesterified Ricinoleic Acid, 38 Polyglycerol Polyricinoleate, 38 *Polyglycerol Polyricinoleic Acid, 38 *Pork Collagen, 39 Potassium Biphosphate, 40 Potassium Dihydrogen Phosphate, 40 Potassium Phosphate, Monobasic, 40 Potassium Phosphate, Tribasic, 41 Potassium Pyrophosphate, 41 Potassium Sorbate, 42 Potassium Triphosphate, 43 Potassium Tripolyphosphate, 43 l-Proline, 43 n-Propanol, 86 Propenylguaethol, 86 Propyl Acetate, 86 n-Propyl Acetate, 86 Propyl Alcohol, 86 Propyl Propionate, 88 n-Propyl Propionate, 88 Protease (Aspergillus niger var.), 20 Protease (Aspergillus oryzae var.), 21 L-2-Pyrrolidinecarboxylic Acid, 43
Index / 115
Q Quimociac TS (Solutions and Indicators), 110 Quinine Hydrochloride, 44
Superglycerinated Fully Hydrogenated Rapeseed Oil, 45 Synthetic Amorphous Silica, 51
T R Rapeseed Oil, Fully Hydrogenated, 44 Rapeseed Oil, Superglycerinated, 45 Rennet, Bovine, 18 Rennet, Calf, 18 Rennet, Microbial (Endothia parasitica), 21 Rennet, Microbial (nonpathogenic strain of Bacillus cereus), 21 Rennet, Microbial (Rhizomucor (Mucor) sp.), 21
S SAIB, 60 *Salatrim, 46, 101 DL-Serine, 50 L-Serine, 50 Short- and Long-Chain Acyl Triglyceride Molecules, 46 Silicon Dioxide, 51 Sodium Acid Pyrophosphate, 52 Sodium Biphosphate, 54 Sodium Carboxymethylcellulose, 11 Sodium Hexametaphosphate, 55 Sodium Hydroxide, 1 N (Solutions and Indicators), 110 Sodium Metaphosphate, Insoluble, 52 Sodium Phosphate, Dibasic, 53 Sodium Phosphate, Monobasic, 54 Sodium Phosphate, Tribasic, 54 Sodium Polyphosphates, Glassy, 55 Sodium Potassium Tripolyphosphate, 56 Sodium Tetrapolyphosphate, 55 Sodium Trimetaphosphate, 56 Sodium Triphosphate, 57 Sodium Tripolyphosphate, 57 *Solin Oil, 58 Solutions and Indicators, 110 Acetic Acid TS, Strong, 110 Nickel Standard Solution, 110 Quimociac TS, 110 Sodium Hydroxide, 1 N, 110 Sorbic Acid, 59 *Soy Protein Concentrate, 59 *Sucrose Acetate Isobutyrate, 60, 101 Sulfurol, 84 Sunset Yellow FCF, 29
Tartrazine, 28 Terpinen-4-ol, 88 ␣-Terpineol, 88 Terpinyl Acetate, 88 Terpinyl Propionate, 88 Tetrapotassium Pyrophosphate, 41 Thiobismethane, 70 L-Threonine, 60 Triacetin, 61 Tribasic Potassium Phosphate, 41 Tribasic Sodium Phosphate, 54 2-Tridecenal, 88 Trimethylamine, 88 2,6,6-Trimethylbicyclo(3.1.1)hept-2-ene, 86 3,7,11-Trimethyl-1,6,10-dodecatrien-3ol, 84 3,7,11-Trimethyl-2,6,10-dodecatrien-1ol, 74 3,5,5-Trimethyl Hexanal, 88 2,3,5-Trimethylpyrazine, 90 Triphosphate, 57 Tripotassium Phosphate, 41 Trisodium Dipotassium Tripolyphosphate, 56 Trisodium Phosphate, 54 Trypsin, 18
U 1,3,5-Undecatriene, 90 (E)-2-Undecenol, 90 trans-2-Undecenol, 90
V L-Valine, 62 Veratraldehyde, 90 Veratryl Aldehyde, 90
W Wool Fat, 31
Z Zingerone, 90
Cumulative Index, FCC IV, Supplement 1, Supplement 2, and Supplement 3 Titles of monographs in Section 2 and those of flavor chemicals in Section 3 are shown in boldface type.
A Abbreviations, 6, 7 Absolute Alcohol, 849 Acacia, 9 “Accurately,” Defined, xxiii Acesulfame K, 10 Acesulfame Potassium, 10 Acetal, (S3)64 Acetaldehyde, 450, 604 Acetaldehyde Diethyl Acetal, (S3)64, 94 Acetaldehyde Test Paper, 861 Acetals, 815 Acetanisole, 450, 680 Acetate Identification Test, 753 Aceteugenol, 498 Acetic Acid, Glacial, 10, 849 Acetic Acid TS, Diluted, 849 Acetic Acid TS, Strong, 848, (S3)110 Acetic Aldehyde, 450 Acetoacetic Ester, 484, (S3)72 Acetoin, 450, 681, (S3)64 2-Acetonaphthone, 530 α-Acetolactatedecarboxylase (Bacillus subtilis containing a Bacillus brevis gene), (S3)19 ␣-Acetolactatedecarboxylase Activity, (S3)104 Acetone, 11 Acetone Peroxides, 12 Acetophenone, 450, 570, 644 N-Acetyl-L-2-amino-4-(methylthio)butyric Acid, 13 4-Acetylanisole, 450 Acetylated Distarch Adipate, 159 Acetylated Distarch Phosphate, 160 Acetylated Mono- and Diglycerides, 12 Acetylated Monoglycerides, 12 Acetylbenzene, 450 3-Acetyl-2,5-dimethylfuran, 450, 644, (S1)58 Acetyl Eugenol, 498
Acetyl Groups, 836 N-Acetyl-l-Methionine, 13 Acetyl Methyl Carbinol, 450, (S3)64 3-Acetyl-6-methyl-1,2-pyran-2,4(3H)dione, 115 Acetyl Propionyl, 544 2-Acetylpyrazine, 450, 604 3-Acetylpyridine, 450, 604, (S1)58 2-Acetylpyrrole, 450, (S3)64 2-Acetyl Thiazole, (S3)64, 94 Acetyl Value, 820 Achilleic Acid, 15 Acid Calcium Phosphate, 68, (S1)9, (S2)4 Acid Ferric Sulfate TS, 852 Acid Hydrolysates of Proteins, 13, (S1)1 Acid-Hydrolyzed Milk Protein, 13, (S1)1 Acid-Hydrolyzed Proteins, 13, (S1)1 Acidified Sodium Chlorite Solutions, (S3)3 Acid-Insoluble Ash, 748 Acidity Determination by Iodometric Method (Flavor Chemicals), 565 Acid-Modified Starch, 159 Acid Number (Rosins and Related Substances), 832 Acid Phosphatase Activity, 788, 789 Acid Phthalate Buffer, 848 Acid Value (Essential Oils and Flavors), 815, (S1)168, (S1)106 Acid Value (Fats and Related Substances), 820 Acid Value (Flavor Chemicals), 568 Acknowledgments, xvii–xviii Aconitic Acid, 15 Activated Carbon, 85, (S1)115 Added Substances Policy, 2 Adipic Acid, 16 Agar, 17 dl-Alanine, 18 l-Alanine, 18 Alcohol, 136, 849 Alcohol, Absolute, 849
117
Alcohol, Aldehyde-Free, 849 Alcohol, Anhydrous, 849 Alcohol, Dehydrated, 849 Alcohol, Diluted, 849 Alcohol, 70%, 849 Alcohol, 80%, 849 Alcohol, 90%, 849 Alcohol C-6, 506, (S3)76 Alcohol C-8, 542 Alcohol C-9, 540 Alcohol C-10, 476 Alcohol C-11, 562 Alcohol C-12, 518 Alcohol Content of Ethyl Oxyhydrate (Flavor Chemicals), 585 Alcoholic Ferric Chloride TS, 852 Alcoholic Potassium Hydroxide, 0.5 N, 854 Alcoholic Potassium Hydroxide TS, 849, 854 Alcoholic Sulfuric Acid, 0.5 N, 859 Alcoholic Sulfuric Acid, 5 N, 859 Alcohols, Total, 815 ALDC Activity, (S3)110 Aldehyde C-6, 504 Aldehyde C-7, 502, (S3)76 Aldehyde C-8, 540 Aldehyde C-9, 538 Aldehyde C-10, 476 Aldehyde C-11 Undecyclic, 560 Aldehyde C-11 Undecylenic, 560 Aldehyde C-12, 518 Aldehyde C-12 MNA, 534 Aldehyde C-14 Pure, So-Called, 560 Aldehyde C-16, 492 Aldehyde C-18, So-Called, 538 Aldehyde-Free Alcohol, 849 Aldehydes and Ketones, 816 Hydroxylamine Method, 816 Hydroxylamine/Tert-Butyl Alcohol Method, 816 Neutral Sulfite Method, 817
118 / Cumulative Index
Algin, 24, 54, 312, 351 Alginates Assay, 768 Algin Derivative, 331 Alginic Acid, 19 Alkaline Borate Buffer, 848 Alkaline Cupric Citrate TS, 851 Alkaline Cupric Tartrate TS, 849 Alkaline Mercuric-Potassium Iodide TS, 850 Allspice Oil, 294 Allura Red AC, 144, (S3)27 p-Allylanisole, 484 Allyl Caproate, 452 Allyl Cyclohexanepropionate, 452, 645 Allyl-3-cyclohexanepropionate, 452 4-Allyl-1,2-dimethoxy Benzene, 530 4-Allylguaiacol, 496 Allyl Heptanoate, 452, 605 Allyl Heptoate, 452 Allyl Hexanoate, 452, 645 Allyl Ionone, 452 Allyl ␣-Ionone, 452, 645 Allyl Isopentanoate, 452 Allyl Isothiocyanate, 452, 568, 681, (S3)64 Allyl Isovalerate, 452, 605, (S1)58 4-Allyl-2-methoxyphenol, 496 4-Allyl-2-methoxyphenol Acetate, 498 Allyl Phenoxy Acetate, (S3)64, 95 Allyl Propionate, (S3)66, 95 Almond Oil, Bitter, FFPA, 19, 573 Alpha-Acetolactatedecarboxylase Activity, (S3)104 Alpha-Amylase Activity (Bacterial), 789 Alpha-Amylase Activity (Nonbacterial), 790 Alphazurine 2G, 860 Aluminum Ammonium Sulfate, 20 Aluminum Identification Test, 753 Aluminum Magnesium Silicate, 41 Aluminum Potassium Sulfate, 21 Aluminum Sodium Sulfate, 21 Aluminum Sulfate, 22 Ambrette Seed Liquid, 23 Ambrette Seed Oil, 23, 596 Aminoacetic Acid, 186 N-[4-[[(2-Amino-1,4-dihydro-4-oxo-6pteridinyl)methyl]amino]benzoyl]-Lglutamic Acid, 157 3-Amino-7-dimethylamino-2methylphenazine Chloride, 861 L-2-Aminoglutaramic Acid, 175 L-2-Amino-5-guanidinovaleric Acid, 32, (S3)5 L-2-Amino-5-guanidinovaleric Acid Monohydrochloride, 33 L-2-Amino-3-hydroxybutyric Acid, 413, (S3)60
FCC IV, Supplement 3
4-Amino-3-hydroxybutyric Acid Trimethylbetaine, (S2)5 DL-2-Amino-3-hydroxypropanoic Acid, 346, (S3)50 L-2-Amino-3-hydroxypropanoic Acid, 347, (S3)50 N-[p-[[(2-Amino-4-hydroxy-6pteridinyl)methyl]amino]benzoyl]glutamic Acid, 157 L-α-Amino-4(or 5)-imidazolepropionic Acid, 192 L-α-Amino-4(or 5)-imidazolepropionic Acid Monohydrochloride, 193 DL-α-Amino-3-indolepropionic Acid, 426 L-α-Amino-3-indolepropionic Acid, 427 L-2-Amino-3-mercaptopropanoic Acid Monohydrochloride, 113 L-2-Amino-3-methylbutyric Acid, 429, (S3)62 DL-2-Amino-4-(methylthio)butyric Acid, 251 L-2-Amino-4-(methylthio)butyric Acid, 250 DL-2-Amino-3-methylvaleric Acid, 206, (S3)30 L-2-Amino-3-methylvaleric Acid, 206, (S3)31 DL-2-Amino-4-methylvaleric Acid, 224, (S3)32 L-2-Amino-4-methylvaleric Acid, 224 L-2-Aminopentanedioic Acid, 174, (S1)22 2-Aminopentanedioic Acid Hydrochloride, 174 Aminopeptidase (Leucine) Activity, (S3)105 Aminopeptidase, Leucine (Aspergillus niger var., Aspergillus oryzae var., and other microbial species), (S3)19 DL-α-Amino-β-phenylpropionic Acid, 292 L-α-Amino-β-phenylpropionic Acid, 292 DL-2-Aminopropanoic Acid, 18 L-2-Aminopropanoic Acid, 18 L-α-Aminosuccinamic Acid, 35 DL-Aminosuccinic Acid, 36, (S3)7 L-Aminosuccinic Acid, 37, (S2)1, (S3)7 Ammonia–Ammonium Chloride Buffer TS, 850 Ammoniacal Silver Nitrate TS, 850 Ammonia Detector Tube, 862 Ammoniated Glycyrrhizin, 23 Ammonia TS, 850 Ammonia TS, Stronger, 850 Ammonia Water, Stronger, 850 Ammonium Acetate TS, 850 Ammonium Alginate, 24 Ammonium Alum, 20 Ammonium Bicarbonate, 25 Ammonium Carbonate, 25 Ammonium Carbonate TS, 850
Ammonium Chloride, 26 Ammonium Chloride TS, 850 Ammonium Glutamate, 257 Ammonium Glycyrrhizinate, 257 Ammonium Glycyrrhizinate, Pentahydrate, 257 Ammonium Hydroxide, 26 Ammonium Identification Test, 753 Ammonium Molybdate TS, 850 Ammonium Oxalate TS, 850 Ammonium Phosphate, Dibasic, 27, (S3)4 Ammonium Phosphate, Monobasic, 27, (S3)4 Ammonium Saccharin, 28 Ammonium Standard Solution, 849 Ammonium Sulfanilate TS, 850 Ammonium Sulfate, 28 Ammonium Sulfide TS, 850 Ammonium Thiocyanate, 0.1 N, 856 Ammonium Thiocyanate TS, 850 Amyl Acetate, 510 1-Amyl Alcohol, 454, (S3)66 Amylase, 130, (S3)18 α-Amylase, 132, 786 β-Amylase, 132, 786 Amyl Butyrate, 454, 510, (S3)66 Amyl Caprylate, 454 Amylcinnamaldehyde, 454 ␣-Amylcinnamaldehyde, 454, 605, (S1)58 Amyl Cinnamate, 454, 646, (S1)58 Amyl Formate, 454, 512, (S3)66 Amyl Heptanoate, 454, (S1)58 Amyl Hexanoate, 512 Amyl Isovalerate, 512 Amyl Octanoate, 454, 605, (S1)60 Amyloglucosidase, 798 Amyl Propionate, 454, 606, (S1)60 Amyl Salicylate, 512, (S3)78 Amyl Valerate, 512 Amyl Vinyl Carbinol, 540 Amyris Oil, West Indian Type, 29, 573 Analytical Performance Parameters, xxiii Anethole, 456, 568, 682 trans-Anethole, 456 Aneurine Hydrochloride, 411 Angelica Root Oil, 29, 573 Angelica Seed Oil, 30, 574 Angelica Seed Oleoresin, 391, 392 Anhydride of Menthane 1:8 Diole, 496 Anhydrous Alcohol, 849 Anhydrous Isopropanol, 852 Anhydrous Lanolin, (S3)31 Anhydrous Methanol, 853 Animal Lipase, 787, (S3)18 p-Anisaldehyde, 524 Anise Oil, 30, 572 Anise Oleoresin, 391, 392
FCC IV, Supplement 3
Anisic Alcohol, 456 Anisic Aldehyde, 524 Anisole, 456, 606 Anisyl Acetate, 456, 568, 606 Anisyl Acetone, 524 Anisyl Alcohol, 456, 606 Anisyl Formate, 456, 607 Annatto Extracts, 31 Anthrone TS, (S1)114 Antimony Trichloride TS, 850, 851 APDC Extraction Method, 766 APM, 35, (S1)4 APM–Ace, (S3)5 APO, 32 Apocarotenal, 32 -Apo-8'-Carotenal, 32 Apparatus for Tests and Assays, 4, 727 D-Araboascorbic Acid, 134 L-Arginine, 32, (S3)5 L-Arginine Monohydrochloride, 33 Arsenic Specification, Requirements for Keeping, xv Arsenic Specifications Policy, 2 Arsenic Test, 755 Ascorbic Acid, 33 L-Ascorbic Acid, 33 Ascorbyl Palmitate, 34 Ash (Acid-Insoluble), 748 Ash (Total), 748 L-Asparagine, 35 Aspartame, 35, (S1)4 Aspartame–Acesulfame Salt, (S3)5, 96 DL-Aspartic Acid, 36, (S3)7 L-Aspartic Acid, 37, (S2)1, (S3)7 L-α-Aspartyl-2-methyl ester Compound with 6-Methyl-1,2,3-oxathiazin-4(3H)one 2,2-Dioxide (1:1), (S3)5 N-L-α-Aspartyl-L-phenylalanine 1-Methyl Ester, 35, (S1)4 Assay by Gas Chromatography (Flavor Chemicals), 564 General Method, Nonpolar Column, 564 General Method, Polar Column, 564 Assay by Titrimetric Procedures (Flavor Chemicals), 565 Direct Aqueous Acid–Base Titrations, 565 Direct Aqueous–Alcoholic Acid–Base Titrations, 565 Assays for Certain Aldehydes and Ketones (Flavor Chemicals), 564 Aldehydes—Hydroxylamine Method, 564 Aldehydes—Hydroxylamine/Tert-Butyl Alcohol Method, 564 Ketones—Hydroxylamine Method, 565 Procedure Requiring the Use of Sealed Glass Vials or Ampules, 564
Cumulative Index / 119
Assay Tolerances, Maximum, 6 Atomic Absorption Spectrophotometric Graphite Furnace Method, 763 Atomic Weights and Chemical Formulas, 3 Autolyzed Yeast, (S1)52 Autolyzed Yeast Extract, 442, (S1)53 Azodicarbonamide, 37 Azodicarboxylic Acid Diamide, 37 Azo Violet, 860
B Bacterial Alpha-Amylase Activity, 789 Bacterial (PC) Proteolytic Activity, 811 Baking Soda, 355 Balances and Weights, 729 Balsam Fir Oil, 156 Balsam Peru Oil, 38, 574 Barium Chloride TS, 850 Barium Diphenylamine Sulfonate TS, 850 Barium Hydroxide TS, (S1)114 Barium Hydroxide, 0.2 N, 856 Barium Standard Solution, 849 Basil Oil, Comoros Type, 39, 574 Basil Oil, European Type, 39, 579 Basil Oil, Italian Type, 39 Basil Oil, Réunion Type, 39 Basil Oil Exotic, 39 Basil Oleoresin, 391, 392 Bay Leaf Oil, 217 Bay Oil, 40, 575 BCD, (S1)15 Beeswax, White, 40 Beeswax, Yellow, 41 Beet Fiber, (S1)45 Beet Sugar, 400, (S2)35 Benedict’s Qualitative Reagent, 850, 851 Bentonite, 41 Benzaldehyde, 456, 607 Benzaldehyde Glyceryl Acetal, 456, 607, (S1)60 Benzene (in Paraffinic Hydrocarbon Solvents), 769 Benzidine TS, 850 1,2-Benzisothiazolin-3-one 1,1-Dioxide, 343 1,2-Benzisothiazolin-3-one 1,1-Dioxide Ammonium Salt, 28 1,2-Benzisothiazolin-3-one 1,1-Dioxide Calcium Salt, 71 1,2-Benzisothiazolin-3-one 1,1-Dioxide Sodium Salt, 378 Benzoate Identification Test, 753 1,2-Benzodihydropyrone, 458, 607, (S1)60 Benzoic Acid, 43 Benzophenone, 458, 646, (S1)60 o-Benzosulfimide, 343
Benzoylbenzene, 458 Benzoyl Peroxide, 43 Benzyl Acetate, 458, 570, 608 Benzyl Alcohol, 458, 570, 646 Benzyl Benzoate, 458, 647 Benzyl Butyrate, 458, 647 Benzyl n-Butyrate, 458 Benzyl Cinnamate, 458, 647 Benzyl Formate, 460, 608 Benzyl Isobutyrate, 460, 608 Benzyl Isovalerate, 460, 648, (S1)60 Benzyl 3-Methyl Butyrate, 460 Benzyl 2-Methyl Propionate, 460 Benzyl Phenylacetate, 460, 608 Benzyl Propanoate, 460 Benzyl Propionate, 648 Benzyl Salicylate, 460, 682 Bergamot Oil, Coldpressed, 44, 575 beta Cyclodextrin, (S1)15 Beta-1,3-Glucan, (S3)15 BHA, 44 BHT, 45 Bicarbonate Identification Test, 753 Biotin, 46 D-Biotin, 46 Birch Tar Oil, Rectified, 46, 575 3,3'-Bis-di(carboxymethyl)aminomethylo-cresolsulfonphthalein, 861 3,7-Bis(dimethylamino)phenazathionium Chloride, 860 Bismuth Nitrate TS, 850 Bisulfite Identification Test, 753 Bitter Almond Oil Free from Prussic Acid, 19 Black Pepper Oil, 47, 572, (S1)5 Black Pepper Oleoresin, 391, 392 Blank Tests, 4 Blank Titration, Residual, 4 Bleached Starch, 159 Bleidner Apparatus, (S3)17 Blue Litmus Paper, 861 Bois de Rose Oil, 47, 576 Boric Acid–Potassium Chloride, 0.2 M, 848 Borneol, (S3)66, 96 Bornyl Acetate, 460, 648 l-Bornyl Acetate, 460 Bound Styrene, 782 Bovine Rennet, 133, (S3)18 Brewer’s Yeast, 440 Brilliant Blue FCF, 139, (S3)24 Bromelain, 132, 786, (S3)18 Bromide Identification Test, 753 Brominated Vegetable Oil, 48 Bromine, 0.1 N, 856 Bromine TS, 850 Bromine Water, 850 Bromocresol Blue, 860 Bromocresol Blue TS, 850
120 / Cumulative Index
Bromocresol Green, 860 Bromocresol Green TS, 850 Bromocresol Purple, 860 Bromocresol Purple TS, 850, (S1)116 Bromophenol Blue, 860 Bromophenol Blue TS, 850 Bromothymol Blue, 860 Bromothymol Blue TS, 850 Buffer Solutions, Standard, 848 Butadiene-Styrene 50/50 Rubber, 49, (S2)2 Butadiene-Styrene 75/25 Rubber, 48, (S2)2 Butane, 50 n-Butane, 50 1,4-Butanedicarboxylic Acid, 16 Butanedioic Acid, 397 2,3-Butanedione, 478 1,2,3,4-Butanetetrol, (S2)10 1-Butanol, 462 2-Butanone, 462, 609, (S1)62 Butan-3-one-2-yl Butanoate, 462, 649 (E)-Butenedioic Acid, 164 Butter Starter Distillate, 394 Butyl Acetate, 462, 649 n-Butyl Acetate, 462 Butyl Alcohol, 462, 649, (S1)62 Butyl Aldehyde, 462 Butylated Hydroxyanisole, 44 Butylated Hydroxymethylphenol, 51 Butylated Hydroxytoluene, 45 Butyl Butyrate, 462, 650 n-Butyl n-Butyrate, 462 Butyl Butyryllactate, 462, 609 2-sec-Butyl Cyclohexanone, (S3)66, 97 1,3-Butylene Glycol, 52 tert-Butylhydroquinone, 408 Butyl Isobutyrate, 464, 650 Butyl Isovalerate, 464, 609, (S1)62 Butyl 2-Methyl Butyrate, (S3)66, 97 Butyl Octadecanoate, 464 Butyl Phenylacetate, 464, 609 Butyl Rubber, 205 Butyl Stearate, 464, (S1)62 Butyraldehyde, 464, 565, 610, (S1)62 Butyric Acid, 464, 565, 610, (S3)66 Butyrin, 558 ␥-Butyrolactone, 464, 650, (S1)62 Butyryllactic Acid, Butyl Ester, 462
C Caffeine, 52 Calcium Acetate, 53 Calcium Acid Pyrophosphate, 53 Calcium Alginate, 54 Calcium Ascorbate, 54 Calcium Biphosphate, 68, (S1)9, (S2)4 Calcium Bromate, 55
FCC IV, Supplement 3
Calcium Carbonate, 55 Calcium Chloride, 56, (S1)5 Calcium Chloride, Anhydrous, 56 Calcium Chloride Double Salt of DL- or DCalcium Pantothenate, 66 Calcium Chloride Solution, 57, (S1)6 Calcium Chloride TS, 850 Calcium Citrate, 58, (S2)4 Calcium Disodium Edetate, 59 Calcium Disodium EDTA, 59 Calcium Disodium Ethylenediaminetetraacetate, 59 Calcium Disodium (Ethylenedinitrilo)tetraacetate, 59 Calcium 4-(β,D-Galactosido)-D-gluconate, 63 Calcium Gluconate, 60 Calcium Glycerophosphate, 60 Calcium Hydroxide, 61 Calcium Hydroxide TS, 850 Calcium Hydroxyapatite, 69, (S1)10 Calcium Identification Test, 753 Calcium Iodate, 62 Calcium Lactate, 62 Calcium Lactobionate, 63 Calcium Lignosulfonate, (S1)7 Calcium Oxide, 64 Calcium Pantothenate, 64 D-Calcium Pantothenate, 64 Calcium Pantothenate, Calcium Chloride Double Salt, 66 Calcium Pantothenate, Racemic, 65 Calcium Peroxide, 67 Calcium Phosphate, Dibasic, 67, (S1)8 Calcium Phosphate, Monobasic, 68, (S1)9, (S2)4 Calcium Phosphate, Tribasic, 69, (S1)10 Calcium Propionate, 70 Calcium Pyrophosphate, 70 Calcium Saccharin, 71 Calcium Silicate, 72, (S1)11 Calcium Sorbate, 73 Calcium Stearate, 74 Calcium Stearoyl Lactylate, 74 Calcium Sulfate, 76 Calcium Sulfate TS, 851 Calf Rennet, 129, 788, (S3)18 Camphene, 466 d-Camphor, 466, 610 Cananga Oil, 76, 572 Candelilla Wax, 77, 715 Cane Sugar, 400, (S2)35 Canola Oil, 77, (S3)8 Cantha, 79 Canthaxanthin, 79 Capraldehyde, 476 Capric Acid, 115 Caproic Acid, 504 Caproic Aldehyde, 504
Capryl Alcohol, 542 Caprylic Acid, 271 Caprylic Aldehyde, 540 Capsicum Oleoresin, 391, 392 Caramel, 80 Caramel Color, 80 Caraway Oil, 85, 576 Caraway Oleoresin, 392 Carbamide, 428 Carbohydrase (Aspergillus niger var., including Aspergillus aculeatus), 786, (S3)19 Carbohydrase (Aspergillus oryzae var.), 786, (S3)19 Carbohydrase (Bacillus acidopullulyticus var.), 786, (S3)19 Carbohydrase (Bacillus stearothermophilus), 787, (S3)19 Carbohydrase (Bacillus subtilis containing a Bacillus megaterium α-amylase gene), 786, 787, (S3)19 Carbohydrase (Bacillus subtilis containing a Bacillus stearothermophilus αamylase gene), 786, 787, (S3)19 Carbohydrase (Candida pseudotropicalis), 786, (S3)19 Carbohydrase (Kluyveromyces marxianus var. lactis), 786, (S3)19 Carbohydrase (Martierella vinaceae var. raffinoseutilizer), 786, (S3)19 Carbohydrase (Rhizopus niveus), 786, (S3)19 Carbohydrase (Rhizopus oryzae var.), 786, (S3)19 Carbohydrase (Saccharomyces species), 787, (S3)19 Carbohydrase [(Trichoderma longibrachiatum var.) (formerly reesei)], 787, (S3)20 Carbohydrase and Protease, Mixed (Bacillus licheniformis var.), 131, (S3)20 Carbohydrase and Protease, Mixed (Bacillus subtilis var. including Bacillus amyloliquefaciens), 131, (S3)20 Carbohydrates (Starches, Sugars, and Related Substances), 836 Carbon, Activated, 85, (S1)115 Carbonate Identification Test, 753 Carbon Dioxide, 87, (S1)12 Carbon Dioxide Detector Tube, 862 Carbon Monoxide Detector Tube, 862 o-Carboxybenzeneazodimethylaniline Hydrochloride, 861 (R)-3-Carboxy-2-hydroxy-N,N,Ntrimethyl-1-propanaminium Hydroxide, Inner Salt, (S2)5 [2-Carboxy-β-(N-(b-methoxycarbonyl-2phenyl)ethylcarbamoyl)]ethanaminium
FCC IV, Supplement 3
6-Methyl-4-oxo-1,2,3-oxathiazin-3-ide2,2-dioxide, (S3)5 Cardamom Oil, 88, 576 Cardamom Oleoresin, 392 Carmine, 89, (S3)10 Carminic Acid, 89, (S3)10 Carnauba Wax, 80 L-Carnitine, (S2)5 Carob Bean Gum, 228 Carotene, 90 -Carotene, 90 Carrageenan, xiv, xxxii Carrot Seed Oil, 91, 577 Carr-Price Reagent, 851 Carvacrol, 466, 610 l-Carveol, 466, 611 4-Carvomenthenol, 554, (S3)88 dextro-Carvone, 466 d-Carvone, 466, 651 l-Carvone, 468, 651 levo-Carvone, 468 l-Carvyl Acetate, 468, 611 -Caryophyllene, 468, 611, (S1)64 Cascarilla Oil, 91, 577 Casein and Caseinate Salts, 92, (S1)115 Cassia Oil, 93, 577 Castor Oil, 94 Catalase, 132, 786 Catalase (Aspergillus niger var.), 786, (S3)20 Catalase (bovine liver), 786, (S3)18 Catalase (Micrococcus lysodeikticus), 786, (S3)20 Catalase Activity, 791 Caustic Potash, 318 Caustic Soda, 364 gamma-CD, (S3)16 Cedar Leaf Oil, 94, 577 Cedar Leaf Oil, White, 94 Celery Oleoresin, 392 Celery Seed Oil, 95, 578 Cellulase, 132, 786 Cellulase Activity, 791 Cellulose Gel, 95 Cellulose Gum, 357, (S1)14, (S2)6, (S3)11 Cellulose, Microcrystalline, 95 Cellulose, Modified, (S1)14 Cellulose, Powdered, 96 “Centrifuge,” Defined, 4 Ceric Ammonium Nitrate TS, 851 Ceric Sulfate, 0.01 N, 856 Ceric Sulfate, 0.1 N, 856 Chamomile Oil, English Type, 98, 578 Chamomile Oil, German Type, 98, 578 Chamomile Oil, Hungarian Type, 98 Changes in Format to the Food Chemicals Codex, Fourth Edition, xv Chemical Formulas and Atomic Weights, 3
Cumulative Index / 121
Chemical Tests and Determinations, 753 Chewing Gum Base, 782 Bound Styrene, 782 Molecular Weight, 783 Quinones, 784 Residual Styrene, 784 Total Unsaturation, 785 Chicle, 249 Chicle, Venezuelan, 249 Chilte, 249 China Clay, 207 Chiquibul, 249 Chloride and Sulfate Limit Tests, 757 Chloride Identification Test, 753 Chlorinated Compounds, 817 Chlorine, 99 Chlorine Detector Tube, 862 Chlorine TS, 851 Chlorophyll, 821 Cholalic Acid, 99 Cholecalciferol, 434 Cholic Acid, 99 Choline Bitartrate, 100 Choline Chloride, 101 Chromatography, 729 Column, 730 Gas, 732 High-Pressure Liquid, 734 Thin-Layer, 731 Chromium, 771 Chromotropic Acid TS, 851 Chymosin, 132 Chymosin (Aspergillus niger var. awamori, Escherichia coli K-12, and Kluyveromyces marxianus, each microorganism containing a calf prochymosin gene), 786, (S3)20 Chymotrypsin, 786, (S3)18 Chymotrypsin Activity, 793 Cinene, 518 1,8-Cineol, 496 Cineole, Percentage of, 818 Cinnamal, 468 Cinnamaldehyde, 468, 611 Cinnamic Acid, 468, 565, 612, (S3)66 Cinnamic Alcohol, 470 Cinnamic Aldehyde, 468 Cinnamon Bark Oil, Ceylon Type, 101, 578 Cinnamon Leaf Oil, 102, 579 Cinnamon Oil, 93 Cinnamyl Acetate, 468, 612 Cinnamyl Alcohol, 470, 612 Cinnamyl Anthranilate, xiv, xxxii Cinnamyl Butyrate, 470, 612 Cinnamyl Cinnamate, 470, 613 Cinnamyl Formate, 470, 613 Cinnamyl Isobutyrate, 470, 613 Cinnamyl Isovalerate, 470, 613, (S1)64
Cinnamyl Propionate, 472, 614, (S1)64 cis and trans Changed to (Z) and (E), xvi Citral, 472, 651, (S1)64 Citrate Identification Test, 753 Citric Acid, 102, (S3)12 Citridic Acid, 15 Citronellal, 472, 652, (S1)64 Citronellol, 472, 683 Citronellyl Acetate, 472, 652 Citronellyl Butyrate, 472, 614 Citronellyl Formate, 474, 683 Citronellyl Isobutyrate, 474, 614, (S1)66 Citronellyl Propanoate, 474 Citronellyl Propionate, 474, 652 Citrus Oils, Ultraviolet Absorbance of, 819 Clary Oil, 103, 579 Clary Sage Oil, 103 Clove Bud Oil, 104 Clove Leaf Oil, 104, 579 Clove Oil, 579 Clove Stem Oil, 105, 580 CMC, 357, (S1)14, (S2)6, (S3)11 Coagulated or Concentrated Latices of Vegetable Origin, 249 Cobalt Identification Test, 754 Cobaltous Chloride CS, 741 Cobaltous Chloride TS, 851 Cobalt–Uranyl Acetate TS, 851 Cocoa Butter Substitute, 105, (S3)13 Coconut Oil (Unhydrogenated), 107 Cognac Oil, Green, 108, 580 Cold Test, 821 Color (AOCS-Wesson), 821 Colorimetric Solutions, 848 Colors, F D & C (also see specific color under F D & C), 771 Chromium, 771 Ether Extracts, 771 Leuco Base, 772 Mercury, 772 Total Color, 773, 774 Uncombined Intermediates and Products of Side Reactions, 775 Column Chromatography, 730 Compliance with Federal Statutes, xv Congo Red TS, 851 “Constant Weight,” Defined, 6 Containers, 6, 7 Light-Resistant, 7 Tared, 6 Tight, 7 Well-Closed, 7 “Cool Place,” Defined, 7 Copaiba Oil, 108, 580 Copper Gluconate, 109 Copper Identification Test, 754 Copper Sulfate, 109 Copper Sulfate TS, (S1)114
122 / Cumulative Index
Coriander Oil, 110, 580 Coriander Oleoresin, 392 Cornmint Oil, Partially Dementholized, 250, (S3)34 Corn Oil (Unhydrogenated), 110 Corn Sugar, 118 Corn Syrup, 173, 843, (S2)13 Costus Root Oil, 111, 581 Cottonseed Oil (Unhydrogenated), 111 Cream of Tartar, 312 Cresol Red, 860 Cresol Red-Thymol Blue TS, 851 Cresol Red TS, 851 o-Cresolsulfonphthalein, 860 p-Cresyl Acetate, 474, 568, 684, (S1)66 p-Cresyl Isobutyrate, 558 p-Cresyl Methyl Ether, 524 Criteria for Food Chemicals Codex Grade, xx Crospovidone, 309 Crown Gum, 249 Crude Fat, 836 Crystal Violet, 860 Crystal Violet TS, 851, 853 “CS,” Defined, 848 Cubeb Oil, 112, 581 Cubeb Oleoresin, 392, 393 Cuminal, 474 Cuminaldehyde, 474 Cuminic Aldehyde, 474, 564, 653, (S1)66 p-Cuminic Aldehyde, 474 Cumin Oil, 113, 581 Cumin Oleoresin, 392, 393 Cupric Citrate TS, Alkaline, 850, 851 Cupric Nitrate TS, 851 Cupric Sulfate, 109 Cupric Sulfate CS, 741 Cupric Sulfate Test Paper, 861 Cupric Sulfate TS, 851 Cupric Tartrate TS, Alkaline, 849, 851, 852 Curcumin Content, 829, (S3)109 Curdlan, (S3)15 Cyanocobalamin, 431 Cyanogen Bromide TS, 851 Cyclamen Aldehyde, 474, 653, (S1)66 beta-Cyclodextrin, (S1)15 γ-Cyclodextrin, (S3)16 gamma-Cyclodextrin, (S3)16, 98 1,2,3,5/4,6-Cyclohexanehexol, 201 Cyclohexyl Acetate, 474, (S3)68 Cyclomaltooctaose, (S3)16 Cyclopentadecanolide (S1) 56 Cyclooctaamylose, (S3)16 p-Cymene, 476, 614, (S3)68 L-Cysteine Monohydrochloride, 113 L-Cystine, 114
FCC IV, Supplement 3
D Damar Gum, 114 Damar Resin, 114 Dammar, 114 Dammar Gum, 114 Dammar Resin, 114 Danish Agar, 164 Data Elements Required for Assay Validation, xxvi, xxvii D.E., 120, (S2)8 “Deaerated Water,” Defined, 5 (E),(E)-2,4-Decadienal, 476, 615, (S1)66, (S3)68 trans,trans-2,4-Decadienal, 476, (S3)68 ␦-Decalactone, 474, 615, (S1)68 ␥-Decalactone, 474, 615, (S1)68 d-Decanal, 474 Decanoic Acid, 115 1-Decanol, 476 (E)-2-Decenal, 476, 615, (S1)68, (S3)68 trans-2-Decenal, 476, (S3)68 (Z)-4-Decenal, 478, 616, (S1)68, (S3)68 cis-4-Decenal, 478, (S3)68 1-Decyl Alcohol, 476 Dehydrated Alcohol, 849 Dehydrated Isopropanol, 852 Dehydrated Methanol, 853 Dehydroacetic Acid, 115 Deleted Monographs, xxxii Denigès’ Reagent, 851, 853 Deoxycholic Acid, 116 “Desiccators and Desiccants,” Defined, 4 Desoxycholic Acid, 116 Detector Tubes, 862 Ammonia, 862 Carbon Dioxide, 862 Carbon Monoxide, 862 Chlorine, 862 Hydrogen Sulfide, 862 Nitric Oxide–Nitrogen Dioxide, 862 Sulfur Dioxide, 862 Water Vapor, 862 Devitalized Wheat Gluten, 435 Dexpanthenol, 116 Dextrin, 117, (S1)18 Dextro Calcium Pantothenate, 64 Dextrose, 118 DHA, 115 Diacetyl, 478, 616 Diacetyl Tartaric Acid Esters of Monoand Diglycerides, 119 2,6-Diaminohexanoic Acid Hydrochloride, 229 Diammonium Phosphate, 27, (S3)4 Diastase Activity (Diastatic Power), 793 Diatomaceous Earth, 120, (S2)8 Diatomaceous Silica, 120, (S2)8 Diatomite, 120, (S2)8
Dibasic Ammonium Phosphate, (S3)4 Dibasic Sodium Phosphate, (S3)53 Dibenzyl Ether, 478, 616 Dibromo-o-cresolsulfonphthalein, 860 Dibromothymolsulfonphthalein, 860 2,6-Di-tert-butyl-p-cresol, 45 Dicalcium Phosphate, 67, (S1)8 Dicarbonic Acid, (S1)19 1,6-Dichloro-1,6-dideoxy-α-Dfructofuranosyl-4-chloro-4-deoxy-α-Dgalactopyranoside, 398, (S2)33 1,2-Dichloroethane, 136 Dichloromethane, 253 Dichlorophenol-indophenol TS, (S1)114 Dietary Fiber from Beets, (S1)45 1,2-Di[(1'-ethoxy)ethoxy]propane, 478, (S3)68 Diethylene Imidoxide, 261 Diethylene Oximide, 261 Diethyl Malonate, 478, 684 Diethyl Sebacate, 478, 654 Diethyl Succinate, 478, 685, (S1)68 Dihydroanethole, 552 Dihydrocarveol, 480, (S1)68, (S3)68 d-Dihydrocarvone, 480, (S1)70, (S3)68 Dihydrocoumarin, 458 13α,12α-Dihydroxycholanic Acid, 116 2,7-Dihydroxynaphthalene TS, 851 1,2-Dihydroxypropane, 331 4,4'-Diketo-β-carotene, 79 Dilauryl Thiodipropionate, 121 Dill Herb Oil, American Type, 123 Dill Oil, 123 Dill Oil, Indian Type, 122 Dill Seed Oil, European Type, 122, 581 Dill Seed Oil, Indian, 122, 597 Dill Seed Oil, Indian Type, 122 Dillseed Oleoresin, 392, 393 Dillweed Oil, American Type, 123, 582 Diluted Acetic Acid TS, 849 Diluted Alcohol, 849 Diluted Hydrochloric Acid TS, 852 Diluted Lead Subacetate TS, 852 Diluted Nitric Acid TS, 853 Diluted Sulfuric Acid TS, 855 Dimagnesium Phosphate, 233 1,2-Dimethoxy-4-allylbenzene, 528 3,4-Dimethoxybenzaldehyde, (S1)56, (S3)90 2,5-Dimethyl-3-acetylfuran, 450 p-Dimethylaminoazobenzene, 861 4'-Dimethylaminoazobenzene-4-sodium Sulfonate, 861 5-Dimethylamino-2-styrylethylquinolinium Iodide, 861 Dimethyl Anthranilate, 480, (S1)70 Dimethyl Benzyl Carbinol, 480, 617 Dimethyl Benzyl Carbinyl Acetate, 480, 654
FCC IV, Supplement 3
Dimethyl Benzyl Carbinyl Butyrate, 480, 654, (S1)70, (S3)70 Dimethyl Dicarbonate, (S1)19, (S1)108 Dimethyldiketone, 478 Dimethyl Ester, (S1)19 Dimethylglyoxal, 478 2,6-Dimethyl-5-heptenal, 480, 617 Dimethylketol, 450, (S3)64 Dimethyl Ketone, 11 6,6-Dimethyl-2-methylenebicyclo[3.1.1]heptane, 550 (E)-3,7-Dimethyl-2,6-octadien-1-al, 498 trans-3,7-Dimethyl-2,6-octadien-1-al, 498 3,7-Dimethyl-1,6-octadien-3-ol, 518 (E)-3,7-Dimethyl-2,6-octadien-1-ol, 498 cis-3,7-Dimethyl-2,6-octadien-1-ol, 53 trans-3,7-Dimethyl-2,6-octadien-1-ol, 498 3,7-Dimethyl-1,6-octadien-3-yl Acetate, 860 3,7-Dimethyl-2,6-octadien-1-yl Acetate, 498 3,7-Dimethyl-1,6-octadien-3-yl Benzoate, 498 3,7-Dimethyl-2,6-octadien-1-yl Butyrate, 500 3,7-Dimethyl-1,6-octadien-3-yl Formate, 520 3,7-Dimethyl-2,6-octadien-1-yl Formate, 500 3,7-Dimethyl-2,6-octadien-3-yl Isobutyrate, 860 3,7-Dimethyl-2,6-octadien-1-yl Phenylacetate, 500 3,7-Dimethyl-2,6-octadien-1-yl Propionate, 500 3,7-Dimethyl-2,6-octadien-3-yl Propionate, 520 Dimethyl Octanol, 482 3,7-Dimethyl-1-octanol, 482, 655 3,7-Dimethyl-3-octanol, 556 3,7-Dimethyl-6-octen-1-ol, 472 3,7-Dimethyl-6-octen-1-yl Acetate, 472 3,7-Dimethyl-6-octen-1-yl Butyrate, 472 3,7-Dimethyl-6-octen-1-yl Formate, 474 3,7-Dimethyl-6-octen-1-yl Isobutyrate, 474 3,7-Dimethyl-6-octen-1-yl Propionate, 474 α,α-Dimethylphenethyl Acetate, 480 α,α-Dimethylphenethyl Alcohol, 480 α,α-Dimethylphenethyl Butyrate, 480, (S3)70 Dimethylpolysiloxane, 123, (S2)8 Dimethylpolysiloxane, Viscosity of, 743 2,3-Dimethylpyrazine, 482, 617, (S1)70, (S3)70 2,5-Dimethylpyrazine, 482, 617 2,6-Dimethylpyrazine, 482, 618 Dimethyl Pyrocarbonate, (S1)19
Cumulative Index / 123
2,5-Dimethylpyrrole, 482, 618, (S1)70, (S3)70 Dimethyl Silicone, 123, (S2)8 Dimethyl Succinate, 482, (S3)70 Dimethyl Sulfide, 482, 618, (S3)70 Dioctyl Sodium Sulfosuccinate, 124, (S1)20 1,4-Dioxane Limit Test, 757 Diphenylamine TS, 851 Diphenylcarbazone TS, 851 Diphenyl Ether, (S3)70, 98 Diphenyl Ketone, 458 Diphenyl Oxide, (S3)70 Diphenylthiocarbazone, 860 Dipotassium Monophosphate, 324, (S1)38 Dipotassium Phosphate, 324, (S1)38 α,α'-Dipyridyl TS, 851 Disodium Dihydrogen Pyrophosphate, 350, (S1)39, (S2)30, (S3)52 Disodium Edetate, 125 Disodium EDTA, 125 Disodium EDTA, 0.05 M, 856 Disodium Ethylenediaminetetraacetate, 125 Disodium (Ethylenedinitrilo)tetraacetate, 125 Disodium Guanosine-5'-monophosphate, 126 Disodium Guanylate, 126 Disodium Inosinate, 127, (S2)9 Disodium Inosine-5'-monophosphate, 127, (S2)9 Disodium Monohydrogen Phosphate, 374, (S3)53 Disodium Phosphate, 374, (S3)53 Disodium Pyrophosphate, 350, (S1)39, (S2)30, (S3)52 Disodium Tartrate, 384 Disodium D-Tartrate, 384 Distarch Phosphate, 160 Distillation Range, 727, 737 3,3'-Dithiobis(2-aminopropanoic acid), 114 Dithizone, 860 Dithizone Method, 762 Dithizone TS, 851 DMDC, (S1)19 Docusate Sodium, (S1)20 ␦-Dodecalactone, 484, 618, (S1)72, (S3)70 ␥-Dodecalactone, 484 Dodecanal, 518 Dodecanoic Acid, 218 1-Dodecanol, 518 (E)-2-Dodecen-1-al, 484, 619, (S1)72, (S3)70 trans-2-Dodecen-1-al, 484, (S3)70 Dried Glucose Syrup, 173, (S2)14 “Dried to Constant Weight,” Defined, 6
Dried Yeast, 440 Drop Method, 832 DSS, 124, (S1)20
E Edible Gelatin, 166 Enanthic Alcohol, 502 Enocianina, 187, (S3)29 Enzyme Activity Alpha-Acetolactatedecarboxylase Activity, (S3)104 Acid Phosphatase Activity, 788 Alpha-Amylase Activity (Bacterial), 789 Alpha-Amylase Activity (Nonbacterial), 790 Aminopeptidase (Leucine) Activity, (S3)105 Catalase Activity, 791 Cellulose Activity, 791 Chymotrypsin Activity, 793 Diastase Activity (Diastic Power), 793 α-Galactosidase Activity, 794 β-Glucanase Activity, 795 Glucoamylase Activity (Amyloglucosidase Activity), 798 Glucose Isomerase Activity, 796 Glucose Oxidase Activity, 798 β-D-Glucosidase Activity, 798 Hemicellulase Activity, 799 Invertase Activity, 800 Lactase (Acid) (β-Galactosidase) Activity, 802 Lactase (Neutral) (β-Galactosidase) Activity, 801 Lipase Activity, 803 Lipase/Esterase (Forestomach) Activity, 804 Lipase (Microbial) Activity for Medium- and Long-Chain Fatty Acids, (S3)105 Lysozyme Activity, (S3)106 Maltogenic Amylase Activity, 804 Milk-Clotting Activity, 805 Pancreatin Activity, 805 Pepsin Activity, 807 Phospholipase A2 Activity, 808 Phytase Activity, 808 Plant Proteolytic Activity, 810 Proteolytic Activity, Bacterial (PC), 811 Proteolytic Activity, Fungal (HUT), 812 Proteolytic Activity, Fungal (SAP), 813 Pullulanase Activity, 814 Trypsin Activity, 814 Enzyme Assays, 786 Enzyme-Hydrolyzed (Source) Protein, 282
124 / Cumulative Index
Enzyme-Modified Fat, 128 Enzyme-Modified Fats, (S1)21 Enzyme-Modified Milkfat, 128 Enzyme-Modified (Source) Protein, 282 Enzyme Preparations, 129 Animal-Derived Preparations, 129, (S3)18 Catalase (bovine liver), 129, 786, (S3)18 Chymotrypsin, 129, 786, (S3)18 Lipase, Animal, 129, 787, (S3)18 Lysozyme, (S3)18 Pancreatin, 129, 787, (S3)18 Pepsin, 129, 788, (S3)18 Phospholipase A2, 129, 788, (S3)18 Rennet, Bovine, 129, 133, (S3)18 Rennet, Calf, 129, (S3)18 Trypsin, 129, 788, (S3)18 Plant-Derived Preparations, 130, (S3)18 Amylase, 130, 786, (S3)18 Bromelain, 130, 786, (S3)18 Ficin, 130, 132, 786, (S3)18 Malt, 130, (S3)18 Papain, 130, 787, (S3)18 Microbially Derived Preparations, 130, (S3)19 α-Acetolactedecarboxylase (Bacillus subtilis containing a Bacillus brevis gene), (S3)19 Aminopeptidase, Leucine (Aspergillus niger var., Aspergillus oryzae var., and other microbial species), (S3)19 Carbohydrase (Aspergillus niger var., including Aspergillus aculeatus), 130, 786, (S3)19 Carbohydrase (Aspergillus oryzae var.), 130, 786, (S3)19 Carbohydrase (Bacillus acidopullulyticus), 130, 788, (S3)19 Carbohydrase (Bacillus stearothermophilus), 130, 786, (S3)19 Carbohydrase (Bacillus subtilis containing a Bacillus megaterium α-amylase gene), 131, 786, (S3)19 Carbohydrase (Bacillus subtilis containing a Bacillus stearothermophilus α-amylase gene), 131, 786, (S3)19 Carbohydrase (Candida pseudotropicalis), 130, 787, (S3)19 Carbohydrase (Kluyveromyces marxianus var. lactis), 130, 787, (S3)19 Carbohydrase (Mortierella vinaceae var. raffinoseutilizer), 130, 786, (S3)19
FCC IV, Supplement 3
Carbohydrase (Rhizopus niveus), 130, 786, (S3)19 Carbohydrase (Rhizopus oryzae var.), 131, 786, (S3)19 Carbohydrase (Saccharomyces species), 131, 787, (S3)19 Carbohydrase [(Trichoderma longibrachiatum var.) (formerly reesei)], 131, 786, (S3)20 Carbohydrase and Protease, Mixed (Bacillus licheniformis var.), 131, (S3)20 Carbohydrase and Protease, Mixed (Bacillus subtilis var. including Bacillus amyloliquefaciens), 131, 787, (S3)20 Catalase (Aspergillus niger var.), 131, 786, (S3)20 Catalase (Micrococcus lysodeikticus), 131, 786, (S3)20 Chymosin (Aspergillus niger var. awamori, Escherichia coli K-12, and Kluyveromyces marxianus, each microorganism containing a calf prochymosin gene), 131, 786, (S3)20 Glucose Isomerase (Actinoplanes missouriensis, Bacillus coagulans, Streptomyces olivaceus, Streptomyces olivochromogenes, Microbacteruim arborescens, Streptomyces rubiginosus var., or Streptomyces murinus), 131, 787, (S3)20 Glucose Oxidase (Aspergillus niger var.), 131, 787, (S3)20 Lipase (Aspergillus niger var.), 131, 787, (S3)20 Lipase (Aspergillus oryzae var.), 132, 787, (S3)20 Lipase [(Candida rugosa) (formerly Candida cylindracea)], 132, 787, (S3)20 Lipase (Rhizomucor (Mucor) miehei), 132, 787, (S3)20 Phytase (Aspergillus niger var.), 132, 788, (S3)20 Protease (Aspergillus niger var.), 132, 786, 788, (S3)20 Protease (Aspergillus oryzae var.), 132, 788, (S3)21 Rennet, Microbial (Endothia parasitica), 132, 788, (S3)21 Rennet, Microbial (Rhizomucor (Mucor) sp.), 132, (S3)21 Rennet, Microbial (nonpathogenic strain of Bacillus cereus), 132, 788, (S3)21 Enzyme Preparations Used in Food Processing (Table), 786, 787, 788
Eosin Y TS, 851 1:8-Epoxy-p-menthane, 496 Epsom Salt, 237 Equisetic Acid, 15 Ergocalciferol, 432 Eriochrome Black T, 860 Eriochrome Black TS, 851 Erythorbic Acid, 134 Erythritol, (S2)10 meso-Erythritol, (S2)10 Erythrosine, 143, (S3)26 Essential Oils, Infrared Spectra of, 572, (S3)93 Essential Oils and Flavors, 815 Esters, 817 Ester Determination, 817 Ester Determination (High-Boiling Solvent), 817 Ester Value, 817 Saponification Value, 817 Estragole, 484, 619 Estragon Oil, 407 Ethanal, 450 Ethanol, 136, 849 Ether Extracts, 771 Ethone, 484, 619, (S3)72 p-Ethoxychrysoidin Monohydrochloride, 860 p-Ethoxychrysoidin TS, 851 4'-Ethoxy-2,4-diaminoazobenzene Monohydrochloride, 860 6-Ethoxy-1,2-dihydro-2,2,4trimethylquinoline, 135, (S3)23 3-Ethoxy-4-hydroxybenzaldehyde, 496 1-Ethoxy-2-hydroxy-4-propenylbenzene, 550, (S3)86 Ethoxylated Mono- and Diglycerides, 134 4-(p-Ethoxyphenylazo)-mphenylenediamine Monohydrochloride, 860 Ethoxyquin, 135, (S3)23 Ethyl Acetate, 484, 685, (S1)72 Ethyl Acetoacetate, 484, 655, (S1)72, (S3)72 Ethyl Acrylate, 486, 686 Ethyl Alcohol, 136, 849 Ethyl Alcohol, 136 Ethyl o-Aminobenzoate, 486 Ethyl p-Anisate, 486, 686 Ethyl Anthranilate, 486, 687 Ethyl Benzoate, 486, 655 Ethyl Benzoyl Acetate, 486, (S3)72 Ethyl-(E)-2-butenoate, 486, (S3)72 Ethyl-trans-2-butenoate, 486, (S3)72 Ethyl Butyl Ketone, 502 Ethyl Butyraldehyde, (S1)72 2-Ethylbutyraldehyde, 486, 619 Ethyl Butyrate, 486, 656
FCC IV, Supplement 3
2-Ethylbutyric Acid, 488, 565, 620, (S1)72 Ethyl Caprate, 488 Ethyl Caproate, 490 Ethyl Capronate, 490 Ethyl Caprylate, 494 Ethyl Cellulose, 136 Ethyl Cinnamate, 488, 620 Ethyl Citrate, 426 Ethyl Crotonate, 486, (S3)72 Ethyl Decanoate, 488, 687, (S1)74 2-Ethyl-3,5(6)-dimethylpyrazine, 488, 656, (S1)74 Ethyl Dodecanoate, 492 Ethylene Brassylate, 488, 620, (S3)72 trans-1,2-Ethylenedicarboxylic Acid, 164 Ethylene Dichloride, 137 Ethylene Trichloride, 425 2-Ethyl Fenchol, 488, 656 Ethyl Formate, 488, 565, 657 4-Ethyl Guaiacol, 490, 620 Ethyl Heptanoate, 490, 657 Ethyl Heptoate, 490 Ethyl Hexanoate, 490, 657 2-Ethyl Hexanol, 490, (S3)72 2-Ethyl-1-hexanol, 490, (S3)72 Ethyl 2-Hydroxypropionate, 490, (S3)72 Ethyl Isobutyrate, 490, 621 Ethyl Isovalerate, 490, 658, (S1)72 Ethyl Lactate, 490, 688, (S3)72 Ethyl Laurate, 492, 621 Ethyl Levulinate, 492, 621, (S3)72 Ethyl Malonate, 478 Ethyl Maltol, 138 Ethyl p-Methoxybenzoate, 486 Ethyl 2-Methylbutyrate, 492, (S1)74, (S3)72 Ethyl 3-Methylbutyrate, 490 Ethyl 2-Methylpentanoate, 492, (S3)74 Ethyl Methylphenylglycidate, 492, 658 2-Ethyl-3-methylpyrazine, 492, 658, (S1)74 Ethyl 3-Methylthiopropionate, 492, 621, (S3)74 Ethyl Myristate, 492, 622 Ethyl Nonanoate, 494, 622 Ethyl 9-Octadecenoate, 494 Ethyl Octanoate, 494, 659, (S1)76 Ethyl Octoate, 494 Ethyl Oleate, 494 Ethyl 3-Oxybutanoate, 484, (S3)72 Ethyl Oxyhydrate, 494 Ethyl Pelargonate, 494 Ethyl n-Pentanoate, 496, (S3)74 Ethyl Phenylacetate, 494, 688 Ethyl Phenylglycidate, 494, 689, (S1)76 Ethyl 3-Phenylpropenate, 488 Ethyl Propionate, 494, 659
Cumulative Index / 125
Ethyl Salicylate, 496, 659, (S1)76, (S3)74 Ethyl Sebacate, 478 Ethyl Succinate, 478 Ethyl 10-Undecanoate, 496, (S1)76, (S3)74 Ethyl Valerate, 496, (S3)74 Ethyl Vanillin, 496, 660 Eucalyptol, 496, 622, (S1)76 Eucalyptus Oil, 138, 582 Eugenic Acid, 496 Eugenol, 496, 689 Eugenol Acetate, 498 Eugenyl Acetate, 498, 622, (S1)78 Eugenyl Methyl Ether, 528 Exaltolide, (S1)56 “Excessive Heat,” Defined, 7 Expanded Perlite, 288 Exsiccated Sodium Sulfite, 383
F Farnesol, 498, 690, (S1)78, (S3)74 Fast Green FCF, 141, (S3)25 Fat, Crude, 836 Fats and Related Substances, 820 Fatty Acid Composition, 821, (S2)42 Fatty Acids, Free, 822 F D & C Blue No. 1, 139, (S3)24 F D & C Blue No. 2, 140, (S3)24 F D & C Colors, 771 F D & C Green No. 3, 141, (S3)25 F D & C Red No. 3, 143, (S3)26 F D & C Red No. 40, 144, (S3)27 F D & C Yellow No. 5, 145, (S3)28 F D & C Yellow No. 6, 146, (S1)115, (S3)29 Federal Statutes, Compliance with, xvi Fehling’s Solution, 849, 851, 852 FEMA Numbers, 449 d-Fenchone, (S3)74, 99 Fenchyl Alcohol, (S3)74, 99 Fennel Oil, 147, 572 Fennel Oleoresin, 392, 393 Ferric Ammonium Citrate, Brown, 147 Ferric Ammonium Citrate, Green, 148 Ferric Ammonium Sulfate TS, 852 Ferric Chloride CS, 741 Ferric Chloride TS, 852 Ferric Chloride TS, Alcoholic, 852 Ferric Citrate, (S2)11 Ferric Orthophosphate, 149 Ferric Phosphate, 149 Ferric Pyrophosphate, 150 Ferric Sulfate TS, Acid, 852 Ferrous Ammonium Sulfate, 0.1 N, 857 Ferrous Citrate, (S2)11 Ferrous Fumarate, 151 Ferrous Gluconate, 153
Ferrous Lactate, 154 Ferrous Sulfate, 155, (S1)115 Ferrous Sulfate, Dried, 155 Ferrous Sulfate TS, 852 FHMO, (S2)18 Ficin, 130, 132, 786, (S3)18 Figures, Significant, 5 “Filtration,” Defined, 4 Fir Needle Oil, Canadian Type, 156, 582 Fir Needle Oil, Siberian Type, 156, 583 Fischer-Tropsch Paraffin, 280 Flame Atomic Absorption Spectrophotometric Method, 763 Flavor Chemicals Acetaldehyde, 450 Acetaldehyde Diethyl Acetal, (S3)64 Acetanisole, 450 Acetoin, 450, (S3)64 Acetophenone, 450 3-Acetyl-2,5-dimethyl Furan, 450, (S1)58 2-Acetylpyrazine, 450 3-Acetylpyridine, 450, (S1)58 2-Acetylpyrrole, 450, (S3)64 2-Acetyl Thiazole, (S3)64 Allyl Cyclohexanepropionate, 452 Allyl Heptanoate, 452 Allyl Hexanoate, 452 Allyl α-Ionone, 452 Allyl Isothiocyanate, 452, (S3)64 Allyl Isovalerate, 452, (S1)58 Allyl Phenoxy Acetate, (S3)64 Allyl Propionate, (S3)66 1-Amyl Alcohol, 454, (S3)66 Amyl Butyrate, 454, (S3)66 α-Amylcinnamaldehyde, 454, (S1)58 Amyl Cinnamate, 454, (S1)58 Amyl Formate, 454, (S3)66 Amyl Heptanoate, 454, (S1)58 Amyl Octanoate, 454, (S1)60 Amyl Propionate, 454, (S1)60 Anethole, 456 Anisole, 456 Anisyl Acetate, 456 Anisyl Alcohol, 456 Anisyl Formate, 456 Benzaldehyde, 456 Benzaldehyde Glyceryl Acetal, 456, (S1)60 1,2-Benzodihydropyrone, 458, (S1)60 Benzophenone, 458, (S1)60 Benzyl Acetate, 458 Benzyl Alcohol, 458 Benzyl Benzoate, 458 Benzyl Butyrate, 458 Benzyl Cinnamate, 458 Benzyl Formate, 460 Benzyl Isobutyrate, 460 Benzyl Isovalerate, 460, (S1)60
126 / Cumulative Index
Benzyl Phenylacetate, 460 Benzyl Propionate, 460 Benzyl Salicylate, 460 Borneol, (S3)66 Bornyl Acetate, 460 2-Butanone, 462, (S1)62 Butan-3-one-2-yl Butanoate, 462 Butyl Acetate, 462 Butyl Alcohol, 462, (S1)62 Butyl Butyrate, 462 Butyl Butyryllactate, 462 2-sec-Butyl Cyclohexanone, (S3)66 Butyl Isobutyrate, 464 Butyl Isovalerate, 464, (S1)62 Butyl 2-Methyl Butyrate, (S3)66 Butyl Phenylacetate, 464 Butyl Stearate, 464, (S1)62 Butyraldehyde, 464, (S1)62 Butyric Acid, 464, (S3)66 γ-Butyrolactone, 464, (S1)62 Camphene, 466 d-Camphor, 466 Carvacrol, 466 l-Carveol, 466 d-Carvone, 466 l-Carvone, 468 l-Carvyl Acetate, 468 β-Caryophyllene, 468, (S1)64 Cinnamaldehyde, 468 Cinnamic Acid, 468, (S3)66 Cinnamyl Acetate, 468 Cinnamyl Alcohol, 470 Cinnamyl Butyrate, 470 Cinnamyl Cinnamate, 470 Cinnamyl Formate, 470 Cinnamyl Isobutyrate, 470 Cinnamyl Isovalerate, 470, (S1)64 Cinnamyl Propionate, 472, (S1)64 Citral, 472, (S1)64 Citronellal, 472, (S1)64 Citronellol, 472 Citronellyl Acetate, 472 Citronellyl Butyrate, 472 Citronellyl Formate, 474 Citronellyl Isobutyrate, 474, (S1)66 Citronellyl Propionate, 474 p-Cresyl Acetate, 474, (S1)66 Cuminic Aldehyde, 474, (S1)66 Cyclamen Aldehyde, 474, (S1)66 Cyclohexyl Acetate, 474, (S3)68 p-Cymene, 476, (S3)68 (E),(E)-2,4-Decadienal, 476, (S1)66, (S3)68 δ-Decalactone, 476, (S1)68 γ-Decalactone, 476, (S1)68 Decanal, 476 (E)-2-Decenal, 476, (S1)68, (S3)68 (Z)-4-Decenal, 478, (S1)68, (S3)68 Decyl Alcohol, 476
FCC IV, Supplement 3
Diacetyl, 478 Dibenzyl Ether, 478 1,2-Di[(1'-ethoxy)ethoxy]propane, 478, (S3)68 Diethyl Malonate, 478 Diethyl Sebacate, 478 Diethyl Succinate, 478, (S1)68 Dihydrocarveol, 480, (S1)68, (S3)68 d-Dihydrocarvone, 480, (S1)70, (S3)68 Dimethyl Anthranilate, 480, (S1)70 Dimethyl Benzyl Carbinol, 480 Dimethyl Benzyl Carbinyl Acetate, 480 Dimethyl Benzyl Carbinyl Butyrate, 480, (S1)70, (S3)70 2,6-Dimethyl-5-heptenal, 480 3,7-Dimethyl-1-octanol, 482 2,3-Dimethylpyrazine, 482, (S1)70, (S3)70 2,5-Dimethylpyrazine, 482 2,6-Dimethylpyrazine, 482 2,5-Dimethylpyrrole, 482, (S1)70, (S3)70 Dimethyl Succinate, 482, (S3)70 Dimethyl Sulfide, 482, (S3)70 Diphenyl Ether, (S3)70 δ-Dodecalactone, 484, (S1)72, (S3)70 γ-Dodecalacone, 484 (E)-2-Dodecen-1-al, 484, (S1)72, (S3)70 Estragole, 484 Ethone, 484, (S3)72 Ethyl Acetate, 484, (S1)72 Ethyl Acetoacetate, 484, (S1)72, (S3)72 Ethyl Acrylate, 486 Ethyl p-Anisate, 486 Ethyl Anthranilate, 486 Ethyl Benzoate, 486 Ethyl Benzoyl Acetate, 486, (S3)72 Ethyl-(E)-2-butenoate, 486, (S3)72 2-Ethylbutyraldehyde, 486, (S1)72 Ethyl Butyrate, 486 2-Ethylbutyric Acid, 488, (S1)72 Ethyl Cinnamate, 488 Ethyl Decanoate, 488, (S1)74 2-Ethyl-3,5(6)-dimethylpyrazine, 488, (S1)74 Ethylene Brassylate, 488, (S3)72 2-Ethyl Fenchol, 488 Ethyl Formate, 488 4-Ethyl Guaiacol, 490 Ethyl Heptanoate, 490 Ethyl Hexanoate, 490 2-Ethyl Hexanol, 490, (S3)72 Ethyl Isobutyrate, 490 Ethyl Isovalerate, 490, (S1)74 Ethyl Lactate, 490, (S3)72 Ethyl Laurate, 492 Ethyl Levulinate, 492, (S3)72
Ethyl 2-Methylbutyrate, 492, (S1)74, (S3)72 Ethyl 2-Methylpentanoate, 492, (S3)74 Ethyl Methylphenylglycidate, 492, (S1)74 2-Ethyl-3-methylpyrazine, 492, (S1)74 Ethyl 3-Methylthiopropionate, 492, (S3)74 Ethyl Myristate, 492 Ethyl Nonanoate, 494 Ethyl Octanoate, 494, (S1)76 Ethyl Oleate, 494 Ethyl Oxyhydrate (so-called), 494 Ethyl Phenylacetate, 494 Ethyl Phenylglycidate, 494, (S1)76 Ethyl Propionate, 494 Ethyl Salicylate, 496, (S1)76, (S3)74 Ethyl 10-Undecenoate, 496, (S1)76, (S3)74 Ethyl Valerate, 496, (S3)74 Ethyl Vanillin, 496 Eucalyptol, 496, (S1)76 Eugenol, 496 Eugenyl Acetate, 498, (S1)78 Farnesol, 498, (S1)78, (S3)74 d-Fenchone, (S3)74 Fenchyl Alcohol, (S3)74 Furfural, 498 Furfuryl Alcohol, (S3)74 2-Furyl Methyl Ketone, (S3)74 Fusel Oil, Refined, 498, (S3)76 Geraniol, 498 Geranyl Acetate, 498 Geranyl Benzoate, 498, (S1)78 Geranyl Butyrate, 500 Geranyl Formate, 500 Geranyl Phenylacetate, 500 Geranyl Propionate, 500 Glyceryl Tripropanoate, 500 (E),(E)-2,4-Heptadienal, 500, (S1)78, (S3)76 γ-Heptalactone, 502, (S1)78 Heptanal, 502, (S3)76 2-Heptanone, 502, (S1)80, (S3)76 3-Heptanone, 502, (S1)80 (Z)-4-Hepten-1-al, 502, (S1)80, (S3)76 Heptyl Alcohol, 502 γ-Hexalactone, 502 Hexanal, 504 Hexanoic Acid, 504 (E)-2-Hexen-1-al, 504, (S1)80, (S3)76 (E)-2-Hexen-1-ol, 504, (S1)80 (Z)-3-Hexen-1-ol, 504 (E)-2-Hexenyl Acetate, 504 (Z)-3-Hexenyl Acetate, 504 (Z)-3-Hexenyl Isovalerate, 506, (S1)80, (S3)76 (Z)-3-Hexenyl 2-Methylbutyrate, 506, (S1)82, (S3)76
FCC IV, Supplement 3
n-Hexyl Acetate, 506 Hexyl Alcohol, 506, (S1)82, (S3)76 Hexyl-2-butenoate, 506 α-Hexylcinnamaldehyde, 506, (S1)82 Hexyl Isovalerate, 506, (S1)82, (S3)78 Hexyl 2-Methylbutyrate, 506, (S1)82, (S3)78 Hydroxycitronellal, 508 Hydroxycitronellal Dimethyl Acetal, 508 4-Hydroxy-2,5-dimethyl-3(2H)furanone, 508 6-Hydroxy-3,7-dimethyloctanoic Acid Lactone, 508 4-(p-Hydroxyphenyl)-2-butanone, 508 Indole, 508, (S1)82 α-Ionone, 510 β-Ionone, 510 Isoamyl Acetate, 510, (S1)84 Isoamyl Alcohol, 510, (S1)84, (S3)78 Isoamyl Benzoate, 510, (S1)84, (S3)78 Isoamyl Butyrate, 510, (S1)84, (S3)78 Isoamyl Formate, 512, (S1)84 Isoamyl Hexanoate, 512, (S1)84 Isoamyl Isovalerate, 512, (S1)86 Isoamyl Phenyl Acetate, 512, (S1)86, (S3)78 Isoamyl Salicylate, 512, (S1)86, (S3)78 Isoborneol, 512 Isobornyl Acetate, 514 Isobutyl Acetate, 514 Isobutyl Alcohol, 514, (S1)86 Isobutyl-2-butenoate, 514 Isobutyl Butyrate, 514 Isobutyl Cinnamate, 514, (S1)86, (S3)78 Isobutyl Phenylacetate, 514 Isobutyl Salicylate, 516 Isobutyraldehyde, 516, (S1)86, (S3)78 Isobutyric Acid, 516 Isoeugenol, 516, (S1)88 Isoeugenyl Acetate, 516, (S1)88 Isopropyl Acetate, 516, (S3)80 Isopulegol, 516 Isovaleric Acid, 518 Lauryl Alcohol, 518 Lauryl Aldehyde, 518 Levulinic Acid, 518, (S3)80 d-Limonene, 518 l-Limonene, 518, (S3)80 Linalool, 518 Linalyl Acetate, 520, (S1)88 Linalyl Benzoate, 520 Linalyl Formate, 520 Linalyl Isobutyrate, 520 Linalyl Propionate, 520, (S1)88 Menthol, 522, (S1)88, (S3)80 l-Menthone, 522, (S1)90, (S3)80 dl-Menthyl Acetate, 522, (S1)90, (S3)80
Cumulative Index / 127
l-Menthyl Acetate, 522, (S1)90, (S3)80 2-Mercaptopropionic Acid, 522 p-Methoxybenzaldehyde, 524 2-Methoxy-3(5)-methylpyrazine, 524, (S1)90, (S3)82 4-p-Methoxyphenyl-2-butanone, 524 2-Methoxypyrazine, 524 Methyl Acetate, 524 4-Methyl Acetophenone, 524 p-Methyl Anisole, 524, (S1)90 Methyl Anthranilate, 526, (S1)92 Methyl Benzoate, 526 α-Methylbenzyl Acetate, 526 α-Methylbenzyl Alcohol, 526 2-Methyl Butanal, 526, (S3)82 3-Methyl Butanal, 526, (S3)82 2-Methylbutyl Acetate, 526, (S3)82 2-Methylbutyl Isovalerate, 526, (S3)82 Methyl Butyrate, 528, (S3)82 2-Methylbutyric Acid, 528, (S3)82 α-Methylcinnamaldehyde, 528, (S1)92 Methyl Cinnamate, 528 6-Methylcoumarin, 528 Methyl Cyclopentenolone, 528 Methyl Eugenol, 528, (S1)92 6-Methyl-5-hepten-2-one, 528 Methyl Hexyl Ketone, 530 Methyl Ionones, 530, (S1)92, (S3)82 Methyl Isobutyrate, 530, (S3)82 Methyl Isoeugenol, 530, (S1)92 5-Methyl-2-isopropyl-2-hexenal, 530 Methyl 2-Methylbutyrate, 530 Methyl-3-methylthiopropionate, 530, (S3)82 Methyl beta-Naphthyl Ketone, 530 Methyl 2-Octynoate, 532 2-Methylpentanoic Acid, 532 4-Methylpentanoic Acid, 532, (S1)94 4-Methyl-2-pentanone, 532, (S1)94, (S3)84 2-Methyl-2-pentenoic Acid, 532 Methyl Phenylacetate, 532 Methyl Phenylcarbinyl Acetate, 532 Methyl Propyl 3-Methyl Butyrate, 532, (S3)84 2-Methylpyrazine, 534 Methyl Salicylate, 534 4-Methyl-5-thiazole Ethanol, 534, (S3)84 3-Methylthiopropionaldehyde, 534 2-Methylundecanal, 534 Myrcene, 534 Myristaldehyde, 534 Myristyl Alcohol, 536 Nerol, 536 Nerolidol, 536, (S3)84 Neryl Acetate, 536 (E),(E)-2,4-Nonadienal, 536, (S1)94, (S3)84
(E),(Z)-2,6-Nonadienal, 536, (S1)94, (S3)84 (E),(Z)-2,6-Nonadienol, 536, (S1)94, (S3)84 δ-Nonalactone, 538, (S1)94 γ-Nonalactone, 538 Nonanal, 538 Nonanoic Acid, 538, (S3)84 2-Nonanone, 538 (E)-2-Nonenal, 538, (S1)96, (S3)84 (E)-2-Nonen-1-ol, 538, (S1)96, (S3)86 (Z)-6-Nonen-1-ol, 538, (S1)96, (S3)86 Nonyl Acetate, 540 Nonyl Alcohol, 540 δ-Octalactone, 540 γ-Octalactone, 540 Octanal, 540 3-Octanol, 540, (S1)96, (S3)86 (E)-2-Octen-1-al, 540 1-Octen-3-ol, 540 (Z)-3-Octen-1-ol, 542 1-Octen-3-yl Acetate, 542, (S1)96, (S3)86 1-Octen-3-yl Butyrate, 542, (S1)98, (S3)86 Octyl Acetate, 542 3-Octyl Acetate, 542 Octyl Alcohol, 542 Octyl Formate, 542 Octyl Isobutyrate, 542 ω-Pentadecalactone, (S1)56 2,3-Pentanedione, 544 2-Pentanone, 544, (S1)98 α-Phellandrene, 544 Phenethyl Acetate, 544 Phenethyl Alcohol, 544, (S1)98 Phenethyl Isobutyrate, 544 Phenethyl Isovalerate, 544, (S1)98 2-Phenethyl 2-Methylbutyrate, 546 Phenethyl Phenylacetate, 546, (S1)98 Phenethyl Salicylate, 546 Phenoxyethyl Isobutyrate, 546 Phenylacetaldehyde, 546 Phenylacetaldehyde Dimethyl Acetal, 546 Phenylacetic Acid, 546 Phenylethyl Anthranilate, 548 Phenylethyl Butyrate, 548 3-Phenyl-1-propanol, 548 2-Phenylpropionaldehyde, 548 3-Phenylpropionaldehyde, 548 2-Phenylpropionaldehyde Dimethyl Acetal, 548 3-Phenylpropyl Acetate, 548 α-Pinene, 550, (S3)86 β-Pinene, 550 Piperidine, 550 Piperonal, 550 Propenylguaethol, 550, (S1)98, (S3)86
128 / Cumulative Index
Propionaldehyde, 550 Propyl Acetate, 550, (S3)86 Propyl Alcohol, 552, (S3)86 p-Propyl Anisole, 552, (S1)100 Propyl Propionate, 552, (S3)88 Pyrrole, 552 Rhodinol, 552 Rhodinyl Acetate, 552 Rhodinyl Formate, 552 Santalol, 554 Santalyl Acetate, 554 α-Terpinene, 554 γ-Terpinene, 554 Terpinen-4-ol, 554, (S3)88 α-Terpineol, 554, (S1)100, (S3)88 Terpinyl Acetate, 556, (S1)100, (S3)88 Terpinyl Propionate, 556, (S1)100, (S3)88 Tetrahydrofurfuryl Alcohol, 556 Tetrahydrolinalool, 556 2,3,5,6-Tetramethylpyrazine, 556 Thymol, 556, (S1)100 Tolualdehyde, 558, (S1)102 p-Tolualdehyde, 558 p-Tolyl Isobutyrate, 558, (S1)102 Tributyrin, 558, (S1)102 2-Tridecenal, 558, (S1)102, (S3)88 Trimethylamine, 558, (S3)88 3,5,5-Trimethyl Hexanal, 558, (S3)88 2,4,5-Trimethyl δ-3-Oxazoline, 560 2,3,5-Trimethylpyrazine, 560, (S1)102, (S3)90 δ-Undecalactone, 560, (S1)104 γ-Undecalactone, 560, (S1)104 Undecanal, 560 2-Undecanone, 560 1,3,5-Undecatriene, (S1)56, (S3)90 10-Undecenal, 560 2-Undecenol/(E)-2-Undecenol, 560, (S1)104, (S3)90 Undecyl Alcohol, 562 Valeraldehyde, 562 Valeric Acid, 562, (S1)104 γ-Valerolactone, 562 Vanillin, 562 Veratraldehyde, (S1)56, (S3)90 Zingerone, 562, (S3)90 Flavor Chemicals, Gas Chromatographic (GC) Assay of, 569 Flavor Chemicals, Infrared Spectra of, 571 Flavor Chemicals, Specifications for, 449 Flavor Chemicals, Test Methods for, 564 Flavor Chemicals Policy, 2 Fluoride Limits Guidelines, 2 Fluoride Limit Test, 758, (S3)103 Folacin, 157 Folic Acid, 157 Food Chemicals Codex, Operating Procedures of, xix–xxiii
FCC IV, Supplement 3
Food Chemicals Codex, Organization of, v–vii Food Chemicals Codex, Scope of, xiv Food-Grade Gelatin, 166 Food Starch, Modified, 158 Food Starch-Modified, 158 Food Starch, Unmodified, 161 Formaldehyde TS, 852 Former and Current Titles of Food Chemicals Codex Monographs, xxxi Formic Acid, 162, 565 Formula Weight, xvi Free Fatty Acids, 822 Free Glycerin or Propylene Glycol, 822 Free Phenols, 818 “Fresh,” Defined, for Solutions, 849 Freskomenthe, (S3)66 Fructose, 162, (S2)12 d-Fructose, 162, (S2)12 Fruit Sugar, 162, (S2)12 Fuchsin-Sulfurous Acid TS, 852 Fully Hydrogenated Rapeseed Oil, 336, (S3)44 Fumaric Acid, 161 Functional Use in Foods, 7 Functions of the Committee on Food Chemicals Codex, xiv, xix Fungal (HUT) Proteolytic Activity, 812 Fungal (SAP) Proteolytic Activity, 813 2-Furaldehyde, 498 Furcelleran, 164 Furfural, 498, 660 Furfuryl Alcohol, (S3)74, 100 2-Furyl Methyl Ketone, (S3)74, 100 Fusel Oil, Refined, 498, 623, (S3)76
G 4-O-β-Galactopyranosyl-D-glucose, 212 α-Galactosidase, 132, 786 α-Galactosidase Activity, 794 Galam, (S2)29 Gallic Acid, Propyl Ester, 333 Garlic Oil, 166, 583 Gas Chromatographic (GC) Assay of Flavor Chemicals, 449, 569 Calculations and Methods, 569 GC Conditions for Analysis, 569 GC System Suitability Test Sample, 570 Gas Chromatography, 732 Gaultheria Oil, 437 Gelatin, 166 Gelatinized Starch, 159 Gellan Gum, 169 General Good Manufacturing Practices Guidelines for Food Chemicals, xx, xxi, xxvii, xxviii, xxix General Information, xix
General Provisions and Requirements, xiv, xv, xx, xxii, 1 General Tests and Assays, 723, (S1)109 Geranial, 472 Geraniol, 498, 660 Geranium Oil, Algerian Type, 170, 583 Geranium Oil, East Indian Type, 277 Geranium Oil, Turkish Type, 277 Geranyl Acetate, 498, 661 Geranyl Benzoate, 498, 690, (S1)78 Geranyl Butyrate, 500, 691 Geranyl Formate, 500, 661 Geranyl Phenylacetate, 500, 661 Geranyl Propionate, 500, 622 Gibberellic Acid, 171 Ginger Oil, 171, 583 Ginger Oleoresin, 392, 393 Glassy Sodium Polyphosphates, (S2)31, (S3)55 β-Glucanase, 132, 786 β-Glucanase Activity, 795 D-Glucitol, 388, (S2)32 Glucoamylase, 132, 786 Glucoamylase Activity (Amyloglucosidase Activity), 795 D-Gluconic Acid, Monopotassium Salt, 317 Glucono Delta-Lactone, 172 α-D-Glucopyranosyl-1,4-D-glucitol, (S2)17, (S3)33 Glucose, 118 D-Glucose, 118 Glucose Isomerase (Actinoplanes missouriensis, Bacillus coagulans, Streptomyces olivaceus, Streptomyces olivochromogenes, Microbacteruim arborescens, Streptomyces rubiginosus var., or Streptomyces murinus), 131, 787, (S3)20 Glucose Isomerase Activity, 796 Glucose Oxidase, 133 Glucose Oxidase (Aspergillus niger var.), 131, 787, (S3)20 Glucose Oxidase Activity, 798 Glucose Syrup, 173, 843, (S2)13 Glucose Syrup, Dried, 173, (S2)14 Glucose Syrup Solids, 173, (S2)14 β-D-Glucosidase, 133, 787 β-D-Glucosidase Activity, 798 Gluside, 343 Glutamic Acid, 174, (S1)22 L-Glutamic Acid, 174, (S1)22 L-Glutamic Acid Hydrochloride, 174 L-Glutamine, 175 Glutaral, 175 Glutaraldehyde, 175 Gluten, Wheat, 435 Glycerin, 176 Glycerin or Propylene Glycol, Free, 822
FCC IV, Supplement 3
Glycerol, 176 Glycerol Ester of Gum Rosin, 177, 715 Glycerol Ester of Partially Dimerized Rosin, 178, 716, (S1)22 Glycerol Ester of Partially Hydrogenated Gum Rosin, 178, 716 Glycerol Ester of Partially Hydrogenated Wood Rosin, 178, 716 Glycerol Ester of Polymerized Rosin, 179, 717 Glycerol Ester of Tall Oil Rosin, 179, 717 Glycerol Ester of Wood Rosin, 180, 717 Glycerol Esters of Condensed Castor Oil Fatty Acids, (S3)38 Glyceryl Behenate, 180 Glyceryl-Lacto Esters of Fatty Acids, 181 Glyceryl Monooleate, 182 Glyceryl Monostearate, 183 Glyceryl Palminostearate, (S1)23 Glyceryl Triacetate, 424, (S3)61 Glyceryl Tribehenate, 180 Glyceryl Tributyrate, 558 Glyceryl Tridocosanoate, 180 Glyceryl Tripropanoate, 500 Glyceryl Tristearate, 185, (S1)115 Glycine, 186 Glycocoll, 186 Good Manufacturing Practices Guidelines for Food Chemicals, xxvii Graham’s Salt, 375, (S2)31, (S3)55 Granular Metal Powders, Sieve Analysis of, 752 Granulated Sugar, 400, (S2)35 Grapefruit Oil, Coldpressed, 186, 584 Grapefruit Oil, Expressed, 186 Grape Skin Extract, 187, (S3)29 Guaiac Resin, 189 Guar Gum, 187 Gum Arabic, 9 Gum Ghatti, 188 Gum Guaiac, 189 Gutta hang kang, 249 Gutta Katiau, 249
H Harmonization, International, xv Heavy Metals Limit Policy, (S3)1 Heavy Metals Limit, Reduced, 3 Heavy Metals Test, 567, 760, (S1)760, (S1)112 Helianthin, 861 Heliotropine, 550 Helium, 189 Hemicellulase, 133, 787 Hemicellulase Activity, 799
Cumulative Index / 129
(E),(E)-2,4-Heptadienal, 500, 623, (S1)78, (S3)76 trans, trans-2,4-Heptadienal, 500, (S1)78, (S3)76 ␥-Heptalactone, 502, 662, (S1)78 Heptaldehyde, 502, (S3)76 Heptanal, 502, 691, (S3)76 2-Heptanone, 502, 623, (S1)80, (S3)76 3-Heptanone, 502, 692, (S1)80 (Z)-4-Hepten-1-al, 502, 623, (S1)80, (S3)76 cis-4-Hepten-1-al, 502, (S1)80, (S3)76 Heptyl Alcohol, 502, 692 n-Heptyl-p-hydroxybenzoate, 190 Heptylparaben, 190 Hexadecanoic Acid, 278 2,4-Hexadienoic Acid, 387, (S3)59 2,4-Hexadienoic Acid, Calcium Salt, 73 2,4-Hexadienoic Acid, Potassium Salt, 327, (S3)42 cis-Hexahydro-2-oxo-1Hthieno[3,4]imidazole-4-valeric Acid, 46 Hexahydropyridine, 550 ␥-Hexalactone, 502, 624 Hexaldehyde, 504 Hexamethyl-p-rosaniline Chloride, 860 Hexanal, 504 Hexanedioic Acid, 16 1,2,3,4,5,6-Hexanehexol, 247, 388, (S2)32 Hexanes, 190 Hexanoic Acid, 504, 565, 662 1-Hexanol, 506, (S3)76 (E)-2-Hexen-1-al, 504, (S1)80, (S3)76 trans-2-Hexen-1-al, 504, (S1)80, (S3)76 (E)-2-Hexen-1-ol, 504, 624, (S1)80 trans-2-Hexen-1-ol, 504, (S1)80 (Z)-3-Hexen-1-ol, 504, 624 cis-3-Hexen-1-ol, 504 (E)-2-Hexenyl Acetate, 504, 624 trans-2-Hexenyl Acetate, 504 (Z)-3-Hexen-1-yl Acetate, 504, 625 cis-3-Hexen-1-yl Acetate, 504 (Z)-3-Hexenyl Isovalerate, 506, (S1)80, (S3)76 cis-3-Hexenyl Isovalerate, 506, (S1)80, (S3)76 (Z)-3-Hexenyl 2-Methylbutyrate, 506, (S1)82, (S2)47, (S3)76 cis-3-Hexenyl 2-Methylbutyrate, 506, (S1)82, (S2)47, (S3)76 n-Hexyl Acetate, 506, 625 Hexyl Alcohol, 506, 693, (S1)82, (S3)76 4-Hexyl-1,3-benzenediol, (S1)24 Hexyl-2-Butenoate, 506, 663 ␣-Hexylcinnamaldehyde, 506, 625, (S1)82 Hexyl Isovalerate, 506, (S1)82, (S3)78 Hexyl 2-Methylbutyrate, 506, (S1)82, (S3)78
Hexylresorcinol, (S1)24 4-Hexylresorcinol, (S1)24, (S1)108 High-Fructose Corn Syrup, 191 High-Pressure Liquid Chromatography, 734 L-Histidine, 192 L-Histidine Monohydrochloride, 193 HMO, (S2)18 Hop Oleoresin, 392, 393 Hops Oil, 193, 584 Hortvet-Sellier Method, Modified, 829 Hydratropic Aldehyde, 548 Hydratropic Aldehyde Dimethyl Acetal, 548 Hydrochloric Acid, 194, 852 Hydrochloric Acid (reagent), 848 Hydrochloric Acid, 1 N, 857 Hydrochloric Acid Buffer, 848 Hydrochloric Acid Table, 748 Hydrochloric Acid TS, Diluted, 852 Hydrocinnamaldehyde, 548 Hydrocinnamyl Alcohol, 548 Hydrogenated Glucose Syrup, 238 Hydrogenated Maltose, (S2)17, (S3)33 Hydrogenated Menhaden Oil, (S2)18 Hydrogen Peroxide, 197 Hydrogen Peroxide TS, 852 Hydrogen Sulfide Detector Tube, 862 Hydrogen Sulfide TS, 852 α-Hydro-omega-hydroxypoly(oxyethylene)poly(oxypropylene)(51-57 moles)poly(oxyethylene) Block Copolymer, 295 α-Hydro-omega-hydroxypoly(oxyethylene)poly(oxypropylene)(63-71 moles)poly (oxyethylene) Block Copolymer, 297 Hydrolyzed Plant Protein (HPP), 13, (S1)1 Hydrolyzed (Source) Protein Extract, 13, (S1)1 Hydrolyzed Vegetable Protein (HVP), 13, (S1)1 3-Hydroxy-2-butanone, 138, 450, (S3)64 Hydroxycitronellal, 508, 570, 693 Hydroxycitronellal Dimethyl Acetal, 508, 663 4-Hydroxydecanoic Acid Lactone, 474 4-Hydroxy-2,5-dimethyl-3(2H)furanone, 508, 625 7-Hydroxy-3,7-dimethyl Octanal, 508 7-Hydroxy-3,7-dimethyl Octanal: Acetal, 508 6-Hydroxy-3,7-dimethyloctanoic Acid Lactone, 508 4-Hydroxydodecanoic Acid Lactone, 484 3-Hydroxy-2-ethyl-4-pyrone, 138
130 / Cumulative Index
(2-Hydroxyethyl)trimethylammonium Bitartrate, 100 (2-Hydroxyethyl)trimethylammonium Chloride, 101 Hydroxylamine Hydrochloride, 0.5 N, 857 Hydroxylamine Hydrochloride TS, 852 Hydroxylamine Method, 564, 565 Hydroxylamine/Tert-Butyl Alcohol Method, 564 Hydroxylated Lecithin, 198, (S1)25 Hydroxyl Value, 822 4-Hydroxy-3-methoxybenzaldehyde, 562 4-Hydroxy-3-methylethylbenzene, 490 5-Hydroxy-6-methyl-3,4pyridinedimethanol Hydrochloride, 334 3-Hydroxy-2-methyl-4-pyrone, 240 Hydroxy Naphthol Blue, 860 5-Hydroxynonanoic Acid Lactone, 538 5-Hydroxyoctanoic Acid Lactone, 540 L-β-(p-Hydroxyphenyl)alanine, 427 4-(p-Hydroxyphenyl)-2-butanone, 508, 626 4-Hydroxyphexanoic Acid Lactone, 502 2-Hydroxypropanoic Acid, Monopotassium Salt, 321 2-Hydroxypropanoic Acid, Monosodium Salt, 365 2-Hydroxypropionic Acid, 211 α-Hydroxypropionic Acid, 211 Hydroxypropoxyl Determination, 777 Hydroxypropyl Alginate, 331 Hydroxypropyl Cellulose, 199 Hydroxypropyl Distarch Phosphate, 159 Hydroxypropyl Methylcellulose, 200 Hydroxypropyl Starch, 160 8-Hydroxyquinoline TS, 852 Hydroxysuccinic Acid, 237, (S2)16 5-Hydroxyundecanoic Acid Lactone, 560 Hypophosphite Identification Test, 754
I Identification Specifications, 4 Identification Tests, 753 Acetate, 753 Aluminum, 753 Ammonium, 753 Benzoate, 753 Bicarbonate, 753 Bisulfite, 753 Bromide, 753 Calcium, 753 Carbonate, 753 Chloride, 753 Citrate, 753 Cobalt, 754 Copper, 754 Hypophosphite, 754 Iodide, 754
FCC IV, Supplement 3
Iron, 754 Lactate, 754 Magnesium, 754 Manganese, 754 Nitrate, 754 Nitrite, 754 Peroxide, 754 Phosphate, 754 Potassium, 754 Sodium, 754, 755 Sulfate, 755 Sulfite, 755 Tartrate, 755 Thiosulfate, 755 Zinc, 755 “Ignite to Constant Weight,” Defined, 6 IMP, 370, (S3)52 Indian Gum, 188 Indicator Papers and Test Papers, 861 Indicators, 4, 860 Indicators, Quantity Used, 4 Indigo Carmine, 140, (S3)24 Indigo Carmine TS, 852, 855 Indigotine, 140, (S3)24 Indigotine Disulfonate, 140 Indole, 508, 694, (S1)82 Infrared Spectra, 571, (S1)107, (S3)93 Essential Oils, 572 Flavor Chemicals, 601 Other Substances, 713 Inositol, 201 i-Inositol, 201 meso-Inositol, 201 Insoluble Sodium Metaphosphate, (S3)52 Insoluble Sodium Polyphosphate, 370, (S3)52 International Harmonization, xv Invertase Activity, 800 Invert Sugar, 202, 846, (S2)14 Invert Sugary Assay, 836, (S1)113 Invert Sugar (Carbohydrates), 846, 836 Invert Sugar Syrup, 202, (S2)14 Iodide Identification Test, 754 Iodine, 0.1 N, 857 Iodine TS, 852 Iodine Value, 823 ␣-Ionone, 510, 663 -Ionone, 510, 694 Iron Ammonium Citrate, 147, 148 Iron, Carbonyl, 202 Iron, Electrolytic, 203 Iron, Reduced, 204, (S1)26 Iron (II) 2-Hydroxypropionate, 154 Iron Identification Test, 754 Iron (II) Lactate, 154 Iron Phosphate, 149 Iron Pyrophosphate, 150 Iron Standard Solution, 849 Isoamyl Acetate, 510, 664, (S1)84
Isoamyl Alcohol, 510, (S1)84, (S3)78 Isoamyl Benzoate, 510, 626, (S1)84, (S3)78 Isoamyl Butyrate, 510, 664, (S1)84, (S3)78 Isoamyl Caproate, 512 Isoamyl Caprylate, 454 Isoamyl Cinnamate, 454 Isoamyl Formate, 512, 664, (S1)84 Isoamyl Hexanoate, 512, 695, (S1)84 Isoamyl Isovalerate, 512, (S1)86 Isoamyl Octanoate, 454 Isoamyl Phenyl Acetate, 512, 626, (S1)86, (S3)78 Isoamyl 3-Phenyl Propenate, 454 Isoamyl Propionate, 454 Isoamyl Salicylate, 512, 695, (S1)86, (S3)78 Isoborneol, 512, 626 Isobornyl Acetate, 514, 696 Isobutane, 205 Isobutyl Acetate, 514, 627 Isobutyl Alcohol, 514, 627 Isobutyl-2-butenoate, 514, 665 Isobutyl Butyrate, 514, 665 Isobutyl Cinnamate, 514, 627, (S1)86, (S2)47, (S3)78 Isobutylene–Isoprene Copolymer, 205, 718 Isobutyl Isovalerate, 532, (S3)84 Isobutyl Phenylacetate, 514, 665 Isobutyl Salicylate, 516, 627 Isobutyraldehyde, 516, 565, 628, (S1)86, (S3)78 Isobutyric Acid, 516, 565, 628 Isoestragole, 456 Isoeugenol, 516, 666, (S1)88 Isoeugenyl Acetate, 516, 696, (S1)88 Isoeugenyl Methyl Ether, 530 DL-Isoleucine, 206, (S3)30 L-Isoleucine, 206, (S3)31 Isopropanol, 207, 852 Isopropanol, Anhydrous, 852 Isopropanol, Dehydrated, 852 Isopropyl Acetate, 516, 628, (S3)80 Isopropylacetic Acid, 518 Isopropyl Alcohol, 207, 852 Isopropyl Alcohol, 207, 852 p-Isopropylbenzaldehyde, 474 Isopropylformic Acid, 516 Isopulegol, 516, 666 Isovaleric Acid, 518, 565, 628
J Jelutong, 249 Juniper Berries Oil, 207, 584
FCC IV, Supplement 3
K Kaolin, 208 Karaya Gum, 208 Karite, (S2)29 Karl Fischer Titrimetric Method for Water, 5, 6, 745 Kasal, 353 Kelp, 209 Kjeldahl Method for Nitrogen Determination, 779 Konjac, 210, (S1)27 Konjac Flour, 210, (S1)27 Konjac Gum, 210, (S1)27 Konnyaku, 210, (S1)27
L Labdanum Oil, 211, 584 Labeling, Use of “FCC” in, 2 Labeling Policy, 2 Lactase, 133, 787 Lactase (Acid) (β-Galactosidase) Activity, 802 Lactase (Neutral) (β-Galactosidase) Activity, 801 Lactated Mono-Diglycerides, 181 Lactate Identification Test, 754 Lactic Acid, 211, (S2)47 Lactic Acid Butyl Ester, Butyrate, 462 Lactose, 212, 837 Lactose (Carbohydrates), 837 Lactylated Fatty Acid Esters of Glycerol and Propylene Glycol, 213 Lactylic Esters of Fatty Acids, 215 Lanolin, Anhydrous, 216, (S3)31 Lard (Unhydrogenated), 217 Laurel Leaf Oil, 217, 585 Laurel Leaf Oleoresin, 392, 393 Lauric Acid, 218 Lauryl Alcohol, 518, 629 Lauryl Aldehyde, 518, 697 Lavandin Oil, Abrial Type, 218, 585 Lavender Oil, 219, 585 Lead Acetate Test Paper, 861 Lead Acetate TS, 852 Lead (and Heavy Metals) Limits Policy, 3 Lead Limit, Reduced, 3 Lead Limit Test, 762, (S1)116 APDC Extraction Method, 766 Atomic Absorption Spectrophotometric Graphite Furnace Method, 763 Dithizone Method, 762 Flame Atomic Absorption Spectrophotometric Method, 763, (S1)116 Lead Subacetate TS, 852 Lead Subacetate TS, Diluted, 852 LEAR, 77, (S3)8
Cumulative Index / 131
Leche caspi (sorva), 249 Leche de vaca, 249 Lecithin, 220, (S1)28 Lecithin, Hydroxylated, 198, (S1)25 Legal Status of the Food Chemicals Codex, xvi Lemongrass Oil, 221, 585, (S3)32 Lemon Oil, Coldpressed, 222, 586, (S2)15 Lemon Oil, Desert Type, Coldpressed, 223, 598 Lemon Oil, Distilled, 222, 586 Lemon Oil, Expressed, 222, (S2)15 Lemon Oil Arizona, 223 DL-Leucine, 224, (S3)32 L-Leucine, 224 Leucine Aminopeptidase, (S3)19 Leuco Base, 772 Levocarnitine, (S2)5 Levulinic Acid, 518, 565, 629, (S3)80 Levulose, 162, (S2)12 Light-Resistant Container, 7 Lime, 64 Lime Oil, Coldpressed, 225, (S1)115 Lime Oil, Distilled, 225, 586 Lime Oil, Expressed, 225 Limestone, Ground, 225 “Limit of Quantitation,” Defined, xxv Limit Tests Chloride and Sulfate, 757 1,4-Dioxane, 757 Fluoride, 758, (S3)103 Lead, 762 Mercury, 766 Selenium, 767 Limit Tests (Flavor Chemicals), 566 Antioxidants in Ethyl Acrylate, 566 Heavy Metals, 567, 760 Hydrocarbons in Eugenol, 567 Hydrocyanic Acid in Benzaldehyde, 567 Lead, 567 Methyl Compounds in Ethyl Acetate, 567 Peroxide Value, 567 Readily Carbonizable Substances in Ethyl Acetate, 567 Readily Oxidizable Substances in dlMenthol, 567 Reducing Substances, 568 d-Limonene, 518, 666 l-Limonene, 518, (S3)80 Linaloe Wood Oil, 227, 587 Linalool, 518, 570, 667 Linalool Determination, 818 Linalyl Acetate, 520, 667, (S1)88 Linalyl Benzoate, 520, 697 Linalyl Formate, 510, 629 Linalyl Isobutyrate, 520, 698
Linalyl Propionate, 520, 698, (S1)88 “Linearity,” Defined, xxv Linoleic Acid, 227 Lipase, 133, 787 Lipase (Aspergillus niger var.), 787, (S3)20 Lipase (Aspergillus oryzae var.), 787, (S3)20 Lipase [(Candida rugosa) (formerly Candida cylindracea)], 787, (S3)20 Lipase (Rhizomucor (Mucor) miehei), 787, (S3)20 Lipase, Animal, 129, 787, (S3)18 Lipase Activity, 803 Lipase (Microbial) Activity for Mediumand Long-Chain Fatty Acids, (S3)105 Lipase/Esterase (Forestomach) Activity, 804 Liquid Petrolatum, 256 Listing Substances in the Food Chemicals Codex, Requirements for, xx Lithium Methoxide, 0.1 N, 857 Litmus, 860 Litmus Paper, Blue, 861 Litmus Paper, Red, 862 Litmus TS, 852 Locust Bean Gum, 228 Locust (Carob) Bean Gum, 228 Loss on Drying, 4, 6, 749 Lovage Oil, 228, 587, (S3)33 Low Erucic Acid Rapeseed Oil, 77, (S3)8 Low Linolenic Acid Flaxseed Oil (Unhydrogenated), (S3)58 Low Linolenic Acid Linseed Oil, (S3)58 L-Lysine Monohydrochloride, 229 Lysozyme, (S3)18 Lysozyme Activity, (S3)106
M Mace Oil, 230, 587 Maddrell’s Salt, 370, (S3)52 Magnesia Mixture TS, 852 Magnesium Carbonate, 230 Magnesium Chloride, 231 Magnesium Gluconate, 231 Magnesium Hydroxide, 232 Magnesium Identification Test, 754 Magnesium Oxide, 233 Magnesium Phosphate, Dibasic, 233 Magnesium Phosphate, Dibasic, Mixed Hydrates, (S1)30 Magnesium Phosphate, Dibasic, Trihydrate, (S1)30 Magnesium Phosphate, Tribasic, 234, (S2)15 Magnesium Silicate, 235 Magnesium Silicate, Synthetic, 235 Magnesium Standard Solution, 849
132 / Cumulative Index
Magnesium Stearate, 236 Magnesium Sulfate, 237 Magnesium Sulfate TS, 852 Malachite Green TS, 852 Malic Acid, 237, (S2)16 DL-Malic Acid, 237, (S2)16 Malonic Ester, 478 Malt, 130, (S3)18 Malt Extract, 241 Maltitol, (S2)17, (S3)33 D-Maltitol, (S2)17, (S3)33 Maltitol Syrup, 238 Maltodextrin, 239, 845 Maltogenic Amylase, 133, 787 Maltogenic Amylase Activity, 804 Maltol, 240 Malt Syrup, 241 Mandarin Oil, Coldpressed, 243, 587 Mandarin Oil, Expressed, 243 Manganese (Carbohydrates), 838 Manganese Chloride, 244 Manganese Citrate, (S1)31 Manganese Gluconate, 245 Manganese Glycerophosphate, 245 Manganese Hypophosphite, 246 Manganese Identification Test, 754 Manganese Sulfate, 246 Mannite, 247 Mannitol, 247 D-Mannitol, 247 Marjoram Oil, Spanish Type, 248, 588 Marjoram Oil, Sweet, 248, 588 Marjoram Oleoresin, Sweet, 392, 393 Massaranduba balata, 249 Massaranduba chocolate, 249 Masticatory Substances, Natural, 249 Mayer’s Reagent, 853 Maximum Assay Tolerances, 6 Melting Range (Fats and Related Substances), 824 Melting Range or Temperature (Physical Tests and Determinations), 728, 738 Menhaden Oil, Hydrogenated, (S2)18 Menhaden Oil, Refined, (S2)22 Mentha Arvensis Oil, Partially Dementholized, 250, 588, (S3)34 p-Mentha-1,5-diene, 544 d-p-Mentha-1,8-diene, 518 l-p-Mentha-1,8-diene, 518, (S3)80 p-Mentha-6,8-dien-2-ol, 466 p-Mentha-6,8-dien-2-yl Acetate, 468 Menthane 1:8 Diole, Anhydride of, 496 3-p-Menthanol, 522, (S3)80 l-p-Menthan-3-one, 522, (S3)80 dl-p-Menthan-3-yl Acetate, 522, (S3)80 l-p-Menthan-3-yl Acetate, 522, (S3)80 p-Menth-1-en-8-ol, 554, (S3)88 p-Menth-4-en-3-ol, 516 Menthen-1-yl-8 Acetate, 556, (S3)88
FCC IV, Supplement 3
Menthen-1-yl-8 Propionate, 556, (S3)88 Menthol, 522, 667, (S1)88, (S3)80 l-Menthone, 522, (S1)90, (S3)80 dl-Menthyl Acetate, 522, (S1)90, (S3)80 l-Menthyl Acetate, 522, (S1)90, (S3)80 2-Mercaptopropionic Acid, 522, 565, 629 Mercuric Acetate TS, 853 Mercuric Chloride TS, 853 Mercuric Nitrate, 0.1 M, 857 Mercuric-Potassium Iodide TS, 853 Mercuric-Potassium Iodide TS, Alkaline, 850, 850, 853 Mercuric Sulfate TS, 851, 853 Mercurous Nitrate TS, 853 Mercury Limit Test, 767 Methanol, 251, 853 Methanol, Anhydrous, 853 Methanol, Dehydrated, 853 Methional, 534 DL-Methionine, 250 L-Methionine, 251 p-Methoxyacetophenone, 450 p-Methoxybenzaldehyde, 524, 699 p-Methoxybenzyl Acetate, 456 p-Methoxybenzyl Alcohol, 456 p-Methoxybenzyl Formate, 456 Methoxyl Determination, 778 2-Methoxy-3(5)-methylpyrazine, 524, 668, (S1)90, (S3)82 4-p-Methoxyphenyl-2-butanone, 524, 630 1-(p-Methoxyphenyl)-1-penten-3-one, 484, (S3)72 2-Methoxy-4-propenylphenol, 516 2-Methoxy-4-propenyl Phenyl Acetate, 516 2-Methoxypyrazine, 524, 630 Methyl Acetate, 524, 630 4'-Methyl Acetophenone, 524, 668 Methylacetopyronone, 115 Methyl Alcohol, 251 Methyl Alcohol, 251 p-Methylaminophenol Sulfate TS, 853 Methyl Amyl Ketone, 502, (S3)76 p-Methyl Anisole, 524, 668, (S1)90 Methyl Anthranilate, 526, 669, (S1)92 Methylbenzaldehyde, 558 p-Methylbenzaldehyde, 558 Methyl Benzoate, 526, 630 ␣-Methylbenzyl Acetate, 526, 699 ␣-Methylbenzyl Alcohol, 526, 669 2-Methyl Butanal, 526, (S3)82 3-Methyl Butanal, 526, (S3)82 β-Methyl Butyl Acetate, 510 2-Methylbutyl Acetate, 526, (S3)82 2-Methylbutyl Isovalerate, 526, (S3)82 2-Methylbutyl-3-methylbutanoate, 526, (S3)82
Methyl Butyrate, 528, (S3)82 2-Methylbutyric Acid, 528, 565, 631, (S3)82 Methylcellulose, 252 Methylcellulose, Viscosity of, 743 Methyl Chavicol, 484 ␣-Methylcinnamaldehyde, 528, 631, (S1)92 Methyl Cinnamate, 528, 669 6-Methylcoumarin, 528, 631 Methyl p-Cresol, 524 3-Methylcyclopentane-1,2-dione, 528 Methyl Cyclopentenolone, 528, 631 Methylene Blue, 860 Methylene Blue TS, 853 Methylene Chloride, 253 3,4-(Methylenedioxy)benzaldehyde, 550 Methyl Ester of Rosin, Partially Hydrogenated, 254, 718, (S2)22 Methyl Ethyl Cellulose, 254 Methyl Ethyl Ketone, 462 Methyl Eugenol, 528, 700, (S1)92 Methyl Formate, xiv, xxxii Methyl Glycol, 331 Methyl Heptenone, 528 6-Methyl-5-hepten-2-one, 528, 700 Methyl Heptine Carbonate, 532 Methyl Heptyl Ketone, 538 Methyl Hexyl Ketone, 530, 632 Methyl p-Hydroxybenzoate, 255 Methyl Ionones, 530, (S1)92, (S3)82 Methyl Isobutyl Ketone, 532, (S3)84 Methyl Isobutyrate, 530, 632, (S3)82 Methyl Isoeugenol, 530, 670 d-1-Methyl-4-isopropenyl-6-cyclohexen2-one, 466 l-1-Methyl-4-isopropenyl-6-cyclohexen-2one, 468 5-Methyl-2-isopropyl-2-hexenal, 530, 670 2-Methyl-3-(p-isopropylphenyl)propionaldehyde, 474 Methyl N-Methyl Anthranilate, 480 Methyl 2-Methyl-butanoate, 530 Methyl 2-Methylbutyrate, 530 7-Methyl-3-methylene-1,6-octadiene, 534 d-2-Methyl-5-(1-methylethenyl)cyclohexanone, 480, (S3)68 1-Methyl-4-(1-methylethyl)-1,3cyclohexadiene, 554 1-Methyl-4-(1-methylethyl)-1,4cyclohexadiene, 554 Methyl-3-methylthiopropionate, 530, (S3)82 Methyl -Naphthyl Ketone, 530, 670 Methyl n-Nonyl Acetaldehyde, 534 Methyl Nonyl Ketone, 560 Methyl 2-Octynoate, 532, 671 Methyl Orange, 861
FCC IV, Supplement 3
Methyl Orange TS, 853 Methylparaben, 255 2-Methylpentanoic Acid, 532, 565 4-Methylpentanoic Acid, 532, 565, 632, (S1)94 4-Methyl-2-pentanone, 532, 565, (S1)94, (S3)84 2-Methyl-2-pentenoic Acid, 532, 565, 633 α-Methyl Phenylacetaldehyde, 548 Methyl Phenylacetate, 532, 671 p-Methylphenyl Acetate, 474 Methyl Phenylcarbinol, 526 Methyl Phenylcarbinyl Acetate, 532, 671 Methylphenyl Ether, 456 Methyl Phenyl Ketone, 450 2-Methyl Propanoic Acid, 516 2-Methyl Propanyl Butyrate, 514 Methyl Propyl Ketone, 544 Methyl Propyl 3-Methyl Butyrate, 532, (S3)84 2-Methylpyrazine, 534, 633 Methyl Pyrazinyl Ketone, 450 Methyl Pyridyl Ketone, 450 Methyl 2-Pyrrolyl Ketone, 450, (S3)64 Methyl Red, 861 Methyl Red-Methylene Blue TS, 853 Methyl Red Sodium, 861 Methyl Red TS, 853 Methylrosaniline Chloride TS, 853 Methyl Salicylate, 534, 701 Methyl Sulfide, 482, (S3)70 2-Methyl-3-(3,7,11,15-tetramethyl-2hexadecenyl)-, (S1)47 4-Methyl-5-thiazole Ethanol, 534, (S3)84 3-Methylthiopropionaldehyde, 534 Methyl p-Tolyl Ketone, 524 2-Methylundecanal, 534, 633 Methyl Vanillin, (S1)56, (S3)90 Methyl Violet TS, 853 Methyl Yellow, 861 Mg/Kg and Percent Policy, 3 Microbial Rennet, (S3)21 Microbial Rennet (Endothia parasitica), 132, 788, (S3)21 Microbial Rennet (nonpathogenic strain of Bacillus cereus), 132, 788, (S3)21 Microbial Rennet (Rhizomucor (Mucor) sp.), 132, (S3)21 Microbiological Attributes Policy, 3 Microcrystalline Wax, Refined, 290 Milk-Clotting Activity, 805 Millon’s Reagent, 853 Mineral Oil, White, 256 Mixed Carbohydrase and Protease, 131, (S3)20 Mixed Paraffinic Hydrocarbons, 190
Cumulative Index / 133
“mm of Mercury,” Defined, 4 Modified Cellulose, 199, 254, 357, (S1)14, (S2)6, (S3)11 Modified Cellulose, EC, 136 Modified Cellulose, HPMC, 200 Modified Cellulose, MC, 252 Modified Food Starch, 158 Modified Hortvet-Sellier Method, 829 Modified Schiff’s Reagent, 854 Molar Solutions, 855 Molecular Weight, xvi Monoammonium L-Glutamate, 257 Monoammonium Glutamate Monohydrate, 257 Monoammonium Glycyrrhizinate, 257 Monoammonium Phosphate, 27, (S3)4 Mono- and Diglycerides, 258 Monobasic Calcium Phosphate, (S2)4 Monobasic Potassium Phosphate, 324, (S3)40 Monobasic Potassium Phosphate, 0.2 M, 828 Monobasic Sodium Phosphate, 374, (S3)54 Mono-tert-butylhydroquinone, 408 Monocalcium Phosphate, 68, (S1)9, (S2)4 Monoglyceride Citrate, 259 1-Monoglycerides, 824 Monoglycerides, Total, 824 Monographs, Codex Specifications, 9 Monographs Added to the Food Chemicals Codex, Third Edition, xxxi Monographs Deleted, xxxii Monographs New to the Food Chemicals Codex, Fourth Edition, xxxii Monopotassium D-Gluconate, 317 Monopotassium L-Glutamate, 259 Monopotassium Glutamate Monohydrate, 259 Monopotassium Phosphate, 324, (S1)39, (S3)40 Monosodium Dihydrogen Phosphate, 374, (S3)54 Monosodium L-Glutamate, 260 Monosodium Glutamate Monohydrate, 260 Monosodium Phosphate, 374, (S3)54 Monostearin, 183 Morpholine, 261, 718 MPG, 259 MSG, 260 Murexide Indicator Preparation, 861 Mustard Oil, 261 Myrcene, 534 Myrcia Oil, 40 Myristaldehyde, 534, 564 Myristic Acid, 262 Myristica Oil, 270 Myristyl Alcohol, 536 Myrrh Oil, 262, 588
N 1,4-Naphthalenedione, (S1)47 α-Naphtholbenzein TS, 853 Naphthol Green B, 853, 861 Naphthol Green TS, 853 Natamycin, 263 Natural Rubber (Latex Solids), 249 Natural Terpene Resin, (S2)36 “Negligible,” Defined, 4 Neral, 472 Nerol, 536, 701 Nerolidol, 536, 633, (S3)84 Neryl Acetate, 536, 634 Nessler’s Reagent, 850, 853 Neutralized Phthalate Buffer, 848 Neutral Red, 861 Neutral Red TS, 853 Neutral Sulfite Method, 817 New Monographs in the Food Chemicals Codex, Fourth Edition, xxxii Niacin, 264, (S1)31 Niacinamide, 264, (S1)32 Niacinamide Ascorbate, 265, (S1)33 Nickel, 265, (S2)23 Nickel Catalysts, 265, (S2)23 Nickel Limit Test, (S2)41 Nickel Standard Solution TS, (S3)110 Nicotinamide, 264, (S1)32 Nicotinic Acid, 264, (S1)31 Niger Gutta, 249 Ninhydrin TS, 853, 855 Nisin Preparation, 266 Nispero, 249 Nitrate Identification Test, 754 Nitre Cake, 356 Nitric Acid, 853 Nitric Acid TS, Diluted, 853 Nitric Oxide–Nitrogen Dioxide Detector Tube, 862 Nitrite Identification Test, 754 Nitrogen, 268 Nitrogen Determination, 779 Nitrogen Enriched Air, 268 Nitrogen Oxide, 269 4-(p-Nitrophenylazo) Resorcinol, 860 Nitrous Oxide, 269 (E),(E)-2,4-Nonadienal, 536, 634, (S1)94, (S3)84 trans,trans-2,4-Nonadienal, 536, (S1)94, (S3)84 (E),(Z)-2,6-Nonadienal, 536, 634, (S1)94, (S2)47, (S3)84 trans,cis-2,6-Nonadienal, 536, (S1)94, (S2)47, (S3)84 (E),(Z)-2,6-Nonadienol, 536, 634, (S1)94, (S3)84
134 / Cumulative Index
trans,cis-2,6-Nonadienol, 536, (S1)94, (S3)84 ␦-Nonalactone, 538, 635, (S1)94 ␥-Nonalactone, 538, 702 Nonanal, 538, 635 Nonanoic Acid, 538, 565, (S3)84 1-Nonanol, 540 2-Nonanone, 538, 635 Nonbacterial Alpha-Amylase Activity, 789 (E)-2-Nonenal, 538, 635, (S1)96, (S3)84 trans-2-Nonenal, 538, (S1)96, (S3)84 (E)-2-Nonen-1-ol, 538, 636, (S1)96, (S3)86 trans-2-Nonen-1-ol, 538, (S1)96, (S3)86 (Z)-6-Nonen-1-ol, 538, 636, (S1)96, (S3)86 cis-6-Nonen-1-ol, 538, (S1)96, (S3)86 Nonyl Acetate, 540, 702 Nonyl Alcohol, 540, 703 Normal Solutions, 855 Nutmeg Oil, 270, 589
O (Z),(Z)-9,12-Octadecadienoic Acid, 227 Octadecanoic Acid, 395 Octadecanoic Acid, 1,2,3-Propane Triyl Ester, 185 (Z)-9-Octadecenoic Acid, 271 ␦-Octalactone, 540, 636 ␥-Octalactone, 540, 672 Octanal, 540, 636 Octanoic Acid, 271 1-Octanol, 542 3-Octanol, 540, (S1)96, (S3)86 2-Octanone, 530 (E)-2-Octen-1-al, 540, 637 trans-2-Octen-1-al, 540 1-Octen-3-ol, 540, 637 (Z)-3-Octen-1-ol, 542, 637 cis-3-Octen-1-ol, 542 1-Octen-3-yl Acetate, 542, 672, (S1)96, (S3)86 1-Octen-3-yl Butyrate, 542, 672, (S1)98, (S3)86 Octyl Acetate, 542, 703 3-Octyl Acetate, 542 Octyl Alcohol, 542, 704 Octyl Formate, 542, 704 Octyl Isobutyrate, 542 Octyl 2-Methylpropanoate, 542 “Odorless,” Defined, 4 Oil Content of Synthetic Paraffin, 750 Oil of Frankincense, 272 Oil of Muscatel, 103 Oil of Shaddock, 186 Oleic Acid, 271 Oleoresin Angelica Seed, 391, 392 Oleoresin Anise, 391, 392
FCC IV, Supplement 3
Oleoresin Basil, 391, 392 Oleoresin Black Pepper, 391, 392 Oleoresin Capsicum, 391, 392 Oleoresin Caraway, 392 Oleoresin Cardamom, 392 Oleoresin Celery, 392 Oleoresin Coriander, 392 Oleoresin Cubeb, 392, 393 Oleoresin Cumin, 392, 393 Oleoresin Dillseed, 392, 393 Oleoresin Fennel, 392, 393 Oleoresin Ginger, 392, 393 Oleoresin Hop, 392, 393 Oleoresin Laurel Leaf, 392, 393 Oleoresin Marjoram Sweet, 392, 393 Oleoresin Origanum, 392, 393 Oleoresin Paprika, 392, 393 Oleoresin Parsley Leaf, 392, 393 Oleoresin Parsley Seed, 392, 393 Oleoresin Pimenta Berries, 392, 393 Oleoresin Rosemary, (S1)43 Oleoresin Thyme, 392, 393 Oleoresin Turmeric, 392, 393 Oleoresins, 829 Color Value, 829 Curcumin Content, 829 Piperine Content, 830 Residual Solvent, 830 Scoville Heat Units, 831 Volatile Oil Content, 832 Olestra, (S1)33 Olibanum Oil, 272, 589 Onion Oil, 272, 589 Operating Procedures of the Food Chemicals Codex, xix–xxii Optical (Specific) Rotation, 739 Orange Oil, Bitter, Coldpressed, 273, 590 Orange Oil, Coldpressed, 273, 589 Orange Oil, Distilled, 274, 590 Organization, 571 Organization of the Food Chemicals Codex, 1981–1995, v Origanum Oil, Spanish Type, 274, 590 Origanum Oleoresin, 392, 393 Orris Root Oil, 275, 590 Orthophenanthroline TS, 853 Orthophosphoric Acid, 293, (S1)38 Others Who Provided Assistance, 1981– 1995, x, xi Oxalic Acid, 0.1 N, 857 Oxalic Acid TS, 854 Ox Bile Extract, 275 Oxidized Hydroxypropyl Starch, 159 Oxidized Starch, 159 1:8-Oxido-p-menthane, 496 Oxyethylene Determination, 825 Oxygen Flask Combustion, 727 Oxystearin, 276 Ozone, 277
P Packaging and Storage, 7 Palmarosa Oil, 277, 591 Palmitic Acid, 278 Palmitoyl L-Ascorbic Acid, 34 Palm Kernel Oil (Unhydrogenated), 278 Palm Oil (Unhydrogenated), 279 Pancreatin, 133, 787, (S3)18 Pancreatin Activity, 805 Panthenol, 116 DL-Panthenol, 280 D(+)-Pantothenyl Alcohol, 116 DL-Pantothenyl Alcohol, 280 Pantothenyl Alcohol, Racemic, 280 Papain, 787, (S3)18 Paprika Oleoresin, 392, 393 Paraffin, Synthetic, 280, 719 Paraffin, Synthetic, Oil Content of, 750 Paraffin Wax, Refined, 290 Parsley Herb Oil, 281, 591 Parsley Leaf Oleoresin, 392, 393 Parsley Seed Oil, 282, 591 Parsley Seed Oleoresin, 392, 393 Partial Acid Digest of (Source) Protein, 282 Partial Enzymatic Digest of (Source) Protein, 282 Partially Dementholized Mentha Arvensis Oil, 250, (S3)34 Partially Hydrogenated Methyl Ester of Rosin, (S2)22 Partially Hydrolyzed Proteins, 282 Partially Hydrolyzed (Source) Protein, 282 Participants in Committee Activities and Other Programs, viii, ix Peach Aldehyde, 560 Peanut Oil (Unhydrogenated), 283 Pectinase, 133, 787 Pectins, 283, (S1)35, (S3)35 PEG, 301 Pelargonic Aldehyde, 538 Pendare, 249 Pennyroyal Oil, 286, 591 -Pentadecalactone, (S1)56 Pentaerythritol Ester of Partally Hydrogenated Wood Rosin, 286, 719, (S2)24 Pentaerythritol Ester of Wood Rosin, 287, 719, (S2)24 1,2,3,4,5-Pentahydroxypentane, 439, (S2)38 1,5-Pentanedial, 175 2,3-Pentanedione, 544, 673 Pentanoic Acid, 562 1-Pentanol, 454, (S3)66 2-Pentanone, 544, 673, (S1)98 Pentapotassium Triphosphate, 328, (S3)43
FCC IV, Supplement 3
Pentasodium Triphosphate, 385, (S1)41, (S3)57 1-Pentyl Butyrate, 454, (S3)66 1-Pentyl Formate, 454, (S3)66 Pentyl Heptanoate, 454 Pentyl Hexanoate, 512 Peppermint Oil, 287, 592 Pepsin, 133, 788, (S3)18 Pepsin Activity, 807 (Source) Peptone, 282 Percentage of Cineole, 818 Perchloric Acid, 0.1 N, 857 Perchloric Acid, 0.1 N, in Dioxane, 858 Perillo, 249 Perlite, 288 Perlite, Expanded, 288 Peroxide Identification Test, 754 Peroxide Value, (S2)43, (S3)108 Petitgrain Oil, Paraguay Type, 289, 592 Petrolatum, 289 Petrolatum, White, 289 Petrolatum, Yellow, 289 Petroleum Wax, 290 Petroleum Wax, Synthetic, 291, 720 pH Determination, 740 ␣-Phellandrene, 544, 705 Phenethyl Acetate, 544, 705 2-Phenethyl Acetate, 544 Phenethyl Alcohol, 544, 706, (S1)98 α-Phenethyl Alcohol, 526 Phenethyl Isobutyrate, 544, 637 Phenethyl Isovalerate, 544, 638, (S1)98 2-Phenethyl 2-Methylbutyrate, 546 Phenethyl Phenylacetate, 546, 673, (S1)98 Phenethyl Salicylate, 546, 674 Phenolphthalein, 861 Phenolphthalein Paper, 862 Phenolphthalein TS, 854 Phenol Red, 861 Phenol Red TS, 854 Phenols, 818 Phenols, Free, 818 Phenolsulfonphthalein, 861 Phenolsulfonphthalein TS, 854 Phenoxyethyl Isobutyrate, 546, 674 Phenylacetaldehyde, 546, 674 Phenylacetaldehyde Dimethyl Acetal, 546, 706 Phenylacetic Acid, 546, 565, 638 DL-Phenylalanine, 292 L-Phenylalanine, 292, (S3)5 Phenyl Carbinol, 458 α-Phenyl Ethyl Acetate, 532 2-Phenylethyl Alcohol, 544 Phenylethyl Anthranilate, 548, 638 Phenylethyl Butyrate, 548, 638 p-Phenylphenol TS, 854 3-Phenyl-1-propanol, 548, 707
Cumulative Index / 135
3-Phenylpropenoic Acid, 468, (S3)66 2-Phenylpropionaldehyde, 548, 707 3-Phenylpropionaldehyde, 548, 675 2-Phenylpropionaldehyde Dimethyl Acetal, 548, 708 3-Phenylpropyl Acetate, 548, 639 Phenylpropyl Alcohol, 548 Phenylpropyl Aldehyde, 548 pH Indicators, 740 PHMO, (S2)18 Phosphate Buffer, 848 Phosphated Distarch Phosphate, 160 Phosphate Identification Test, 754 Phosphate Standard Solution, 849 Phospholipase A2, 133, 788, (S3)18 Phospholipase A2 Activity, 808 Phosphoric Acid, 293, 854, (S1)38 Phosphoric Acid, 854 Phosphorus (Carbohydrates), 838 Phosphotungstic Acid TS, 854 Phylloquinone, (S1)47 Physical Tests and Determinations, 729 Physicochemical Properties, 737 Phytase, 133, 788 Phytase (Aspergillus niger var.), 788, (S3)20 Phytase Activity, 808 Phytonadione, (S1)47 Picric Acid TS, 854, 855 Pimaricin, 263 Pimenta Berries Oil, 294 Pimenta Berries Oleoresin, 392, 393 Pimenta Leaf Oil, 293, 592 Pimenta Oil, 294, 592 Pimento Leaf Oil, 293 Pimento Oil, 294 ␣-Pinene, 550, (S3)86 -Pinene, 550 2-Pinene, 550, (S3)86 l-α-Pinene, 550, (S3)86 Pine Needle Oil, 156, 294 Pine Needle Oil, Dwarf, 294, 599 Pine Needle Oil, Scotch Type, 295, 599 Piperidine, 550, 639 Piperine Content, 830 Piperonal, 550, 675 Piperonyl Aldehyde, 550 Plant Proteolytic Activity, 810 Platinum-Cobalt CS, 741 Policies and Guidelines, 1 Added Substances Policy, 2 Arsenic Specifications Policy, 2 FCC Substances Containing Sulfur Dioxide Policy, 2 Flavor Chemicals Policy, 2 Fluoride Limits Guidelines, 2 General Policy, 1 Labeling Policy, 2
Lead (and Heavy Metals) Limits Policy, 3 Mg/Kg and Percent Policy, 3 Microbiological Attributes Policy, 3 Poloxamer 331, 295 Poloxamer 407, 497 Polydextrose, 297, (S2)24 Polydextrose Solution, 300 Polydimethylsiloxane, 123, (S2)8 Polyethylene, 301, 721, 783 Polyethylene Glycols, 301 Polyglycerate (60), 134 Polyglycerol Esters of Fatty Acids, 303 Polyglycerol Esters of Interesterified Ricinoleic Acid, (S3)38 Polyglycerol Polyricinoleate, (S3)38 Polyglycerol Polyricinoleic Acid, (S3)38 Polyisobutylene, 304, 721, 783, (S2)27 Poly[1-(2-oxo-1-pyrrolidinyl)ethylene], 310 Poly(oxy-1,2-ethanediyl) Derivative, 306, 307, 308 Polyoxyethylene (20) Mono- and Diglycerides of Fatty Acids, 134 Polyoxyethylene (20) Sorbitan Monolaurate, 306 Polyoxyethylene (20) Sorbitan Monooleate, 308 Polyoxyethylene (20) Sorbitan Monostearate, 307 Polyoxyethylene (20) Sorbitan Tristearate, 307 Polypropylene Glycol, 305 Polysorbate 20, 306 Polysorbate 60, 307 Polysorbate 65, 307 Polysorbate 80, 308 Polyvinyl Acetate, 309, 721, 783 Polyvinylpolypyrrolidone, 309 Polyvinylpyrrolidone, 310 Pork Collagen, (S3)39 Potassium Acetate TS, 854 Potassium Acid Phthalate, 0.1 N, 858 Potassium Acid Tartrate, 312 Potassium Alginate, 312 Potassium Alum, 21 Potassium Benzoate, 313 Potassium Bicarbonate, 313 Potassium Biphosphate, 324, (S1)39, (S3)40 Potassium Biphthalate, 0.2 M, 848 Potassium Bitartrate, 312 Potassium Bromate, 314 Potassium Carbonate, 314 Potassium Carbonate Solution, 315 Potassium Chloride, 315 Potassium Chloride, 0.2 M, 848 Potassium Chromate TS, 854 Potassium Citrate, 316
136 / Cumulative Index
Potassium Dichromate, 0.1 N, 858 Potassium Dichromate TS, 854 Potassium Dihydrogen Phosphate, 324, (S1)39, (S3)40 Potassium Ferricyanide TS, 854 Potassium Ferrocyanide TS, 854 Potassium Gibberellate, 316 Potassium Gluconate, 317 Potassium Glutamate, 259 Potassium Glycerophosphate, 318 Potassium Hydroxide, 318, 854 Potassium Hydroxide, 0.5 N, Alcoholic, 849 Potassium Hydroxide, 1 N, 858 Potassium Hydroxide Solution, 319 Potassium Hydroxide TS, 854 Potassium Hydroxide TS, Alcoholic, 854 Potassium Identification Test, 754 Potassium Iodate, 319 Potassium Iodate, 0.05 M, 858 Potassium Iodide, 320 Potassium Iodide TS, 854 Potassium Kurrol’s Salt, 325, (S2)28 Potassium Lactate Solution, 321 Potassium Metabisulfite, 322 Potassium Metaphosphate, 325, (S2)28 Potassium Nitrate, 323 Potassium Nitrite, 323 Potassium Permanganate, 0.1 N, 858 Potassium Permanganate TS, 854 Potassium Phosphate, Dibasic, 324, (S1)38 Potassium Phosphate, Monobasic, 324, (S1)39, (S3)40 Potassium Phosphate, Monobasic, 0.2 M, 848 Potassium Phosphate, Tribasic, 325, (S2)28, (S3)41 Potassium Polymetaphosphate, 325, (S2)28 Potassium Pyroantimonate TS, 854 Potassium Pyrophosphate, 326, (S3)41 Potassium Pyrosulfite, 322 Potassium Salt, 7 Potassium Sorbate, 327, (S3)42 Potassium Sulfate, 328 Potassium Sulfate TS, 854 Potassium Sulfite, 328 Potassium Triphosphate, 328, (S3)43 Potassium Tripolyphosphate, 328, (S3)43 Povidone, 310 Precipitated Calcium Phosphate, 69, (S1)10 “Precision,” Defined, xxiii Preface, xiii Procedure for Revising Specifications, xxii
FCC IV, Supplement 3
Procedures for Submission and Development of Specifications, xxi, xxii L-Proline, 329, (S3)43 Propane, 329 1,2-Propanediol, 331 1,2,3-Propanetriol Octadecanoate, 183 2-Propanol, 207, 852 n-Propanol, 552, (S3)86 2-Propanone, 11 p-Propenylanisole, 456 Propenylguaethol, 550, 708, (S1)98, (S3)88 4-Propenyl Veratrole, 530 Propionaldehyde, 550, 565, 639 Propionic Acid, 330, (S1)115 Propyl Acetate, 550, (S3)86 n-Propyl Acetate, 550, 639, (S3)86 Propyl Alcohol, 552, (S3)86 p-Propyl Anisole, 552, 675, (S1)100 Propylene Chlorohydrin (Carbohydrates), 839 Propylene Glycol, 331 Propylene Glycol Alginate, 331 Propylene Glycol Ether of Methylcellulose, 200 Propylene Glycol Lactostearate, 213 Propylene Glycol Mono- and Diesters, 332 Propylene Glycol Mono- and Diesters of Fatty Acids, 332 Propylene Glycol Monostearate, 332 Propyl Gallate, 333 Propyl p-Hydroxybenzoate, 333 Propylparaben, 333 Propyl Propionate, 552, (S3)88 n-Propyl Propionate, 552, 640, (S3)88 Protease, 133, 788 Protease (Aspergillus niger var.), 788, (S3)20 Protease (Aspergillus oryzae var.), 788, (S3)21 Proteolytic Activity, Bacterial (PC), 811 Proteolytic Activity, Fungal (HUT), 812 Proteolytic Activity, Fungal (SAP), 813 Proteolytic Activity, Plant, 810 Pteroylglutamic Acid, 157 Pullulanase, 133, 788 Pullulanase Activity, 814 Purified Oxgall, 275 PVP, 310 PVPP, 309 3-Pyridinecarboxylic Acid, 264, (S1)31 Pyridoxine Hydrochloride, 334 Pyromucic Aldehyde, 498 Pyrrole, 552, 640 L-2-Pyrrolidinecarboxylic Acid, 329, (S3)43
Q Qualitative Test for Phenols Using Ferric Chloride, 568 Quimociac TS, 854, (S3)110 Quinaldine Red, 861 Quinaldine Red TS, 854 Quinine Hydrochloride, 335, (S3)44 Quinine Sulfate, 336 Quinones, 784
R Racemic Pantothenyl Alcohol, 280 “Range,” Defined, xxv Rapeseed Oil, Fully Hydrogenated, 336, (S3)44 Rapeseed Oil, Superglycerinated, 337, (S3)45 Readily Carbonizable Substances, 740 Reagent Solutions, 5, 848 Reagent Specifications, 4 Reagents, Hazardous or Toxic, 5 Red Litmus Paper, 862 Reduced Heavy Metals Limit, 3 Reduced Iron, (S1)26 Reduced Lactose Whey, (S1)50 Reduced Minerals Whey, (S1)51 Reduced Lead Limit, 3 Reducing Sugars Assay, 840 Reference Standards, 5 Refined Bleached Shellac, 348 Refined Menhaden Oil, (S2)22 Refined Microcrystalline Wax, 290 Refined Paraffin Wax, 290 Refined Sheanut Oil, (S2)29 Refractive Index, 741 Regular Bleached Shellac, 347 Reichert-Meissl Value, 826 Rennet, 788 Rennet, Bovine, 133, (S3)18 Rennet, Calf, 129, 133, (S3)18 Rennet, Microbial (Endothia parasitica), 132, 788, (S3)21 Rennet, Microbial (nonpathogenic strain of Bacillus cereus), 132, 788, (S3)21 Rennet, Microbial (Rhizomucor (Mucor) sp.), 132, (S3)21 Requirements for Keeping the Arsenic Specification, 2 Requirements for Listing Substances in the Food Chemicals Codex, xx Residual Blank Titration, 4 Residual Solvent, 830 Residual Styrene, 784 Residue on Evaporation, 819 Residue on Evaporation (Flavor Chemicals), 568 Residue on Ignition (Sulfated Ash), 751
FCC IV, Supplement 3
Revising Specifications, Procedure for, xxii Rhodinol, 552, 676 Rhodinyl Acetate, 522, 709 Rhodinyl Formate, 522, 709 Riboflavin, 338 Riboflavin 5'-Phosphate Ester Monosodium Salt, 339 Riboflavin 5'-Phosphate Sodium, 339 Rice Bran Wax, 341, 722 Ring-and-Ball Method, 834 “Robustness,” Defined, xxvi Rochelle Salt, 376 Rose Geranium Oil, Algerian Type, 170 Rosemary Oil, 341, 593 Rosemary Oleoresin, (S1)43 Rose Oil, 342, 593 Rosidinha, 249 Rosins and Related Substances, 832 Rue Oil, 342, 593 “Ruggedness,” Defined, xxvi Rum Ether, So-Called, 494
S Saccharin, 343 Safflower Oil (Unhydrogenated), 343 Sage Oil, Dalmatian Type, 344, 593 Sage Oil, Spanish Type, 345, 594 SAIB, (S3)60 Salatrim, (S3)46, 101 SALP, 353 Salt, 358 Sandalwood Oil, East Indian Type, 345, 594 Sandalwood Oil, West Indian Type, 29 Santalol, 554, 710 Santalyl Acetate, 554, 676 Saponification Value (Esters) (Essential Oils and Flavors), 817 Saponification Value (Fats and Related Substances), 827 Savory Oil (Summer Variety), 346, 594 Schiff’s Reagent, Modified, 854 Scope of the Food Chemicals Codex, xiv Scoville Heat Units, 831 Selenium Limit Test, 767 DL-Serine, 346, (S3)50 L-Serine, 347, (S3)50 Shea Butter, (S2)29 Sheanut Butter, Refined, (S2)29 Shellac, Bleached, 347 Shellac, Bleached, Wax-Free, 348 Shellac, Refined Bleached, 348 Shellac, Regular Bleached, 347 Shellac, White, 347 Short- and Long-Chain Acyl Triglyceride Molecules, (S3)46
Cumulative Index / 137
Sieve Analysis of Granular Metal Powders, 752 Significant Figures, 5 Silica, Synthetic Amorphous, 348 Silicon Dioxide, 348, (S3)51 Silver Diethyldithiocarbamate Solution, (S2)47 Silver Nitrate, 0.1 N, 858 Silver Nitrate, Ammoniacal, TS, 850 Silver Nitrate TS, 854 Slaked Lime, 61 Smectite, 41 Soap, 827 Soda Alum, 21 Sodium Acetate, 349 Sodium Acetate, 0.1 N, 858 Sodium Acetate, Anhydrous, 350 Sodium Acid Pyrophosphate, 350, (S1)39, (S2)30, (S3)52 Sodium Acid Sulfate, 356 Sodium Acid Sulfite, 356 Sodium Alginate, 351 Sodium Alum, 21 Sodium Aluminosilicate, 351 Sodium Aluminum Phosphate, Acidic, 353 Sodium Aluminum Phosphate, Basic, 353 Sodium Arsenite, 0.05 N, 858 Sodium Ascorbate, 354 Sodium L-Ascorbate, 354 Sodium Benzoate, 355 Sodium o-Benzosulfimide, 378 Sodium Bicarbonate, 355 Sodium Biphosphate, 356, 374, (S3)54 Sodium Bisulfate, 356 Sodium Bisulfite, 346 Sodium Bisulfite TS, 854 Sodium Bitartrate TS, 854 Sodium Borate TS, 854 Sodium Carbonate, 357 Sodium Carbonate TS, 854 Sodium Carboxymethylcellulose, 357, (S1)14, (S2)47, (S3)11 Sodium Carboxymethylcellulose, Viscosity of, 744 Sodium Chloride, 358 Sodium Choleate, 275 Sodium Citrate, 360 Sodium Cobaltinitrite TS, 854 Sodium Dehydroacetate, 361 Sodium Diacetate, 361 Sodium Erythorbate, 362, (S2)30 Sodium Ferric Pyrophosphate, 362 Sodium Ferrocyanide, 363 Sodium Fluoride TS, 854 Sodium Gluconate, 363 Sodium Glutamate, 260 Sodium 5'-Guanylate, 126
Sodium Hexametaphosphate, 375, (S2)31, (S3)55 Sodium Hydrogen Diacetate, 361 Sodium Hydrogen Sulfite, 356 Sodium Hydroxide, 364, 854 Sodium Hydroxide, 1 N, 858, (S3)110 Sodium Hydroxide Solution, 364 Sodium Hydroxide TS, 854 Sodium 3-(1-Hydroxyethylidene)-6methyl-1,2-pyran-2,4(3H)-dione, 361 Sodium 1-(1-Hydroxy-2-naphthylazo)-5nitro-2-naphthol-4-sulfonate, 860 Sodium Hypophosphite, 365, (S2)47 Sodium Hyposulfite, 384 Sodium Identification Test, 754 Sodium Indigotindisulfonate TS, 852, 855 Sodium 5’-Inosinate, 127, (S2) Sodium Iron Pyrophosphate, 362 Sodium Lactate Solution, 365 Sodium Lauryl Sulfate, 367 Sodium Lignosulfonate, (S1)40 Sodium Magnesium Aluminosilicate, 368 Sodium Metabisulfite, 369 Sodium Metaphosphate, Insoluble, 370, (S3)52 Sodium Metasilicate, 370 Sodium Methoxide, 371 Sodium Methoxide, 0.02 N, in Toluene, 859 Sodium Methoxide, 0.1 N, in Pyridine, 859 Sodium Methylate, 371 Sodium Nitrate, 373 Sodium Nitrite, 373 Sodium Nitroferricyanide TS, 855 Sodium Phosphate, Dibasic, 374, (S3)53 Sodium Phosphate, Monobasic, 374, (S3)54 Sodium Phosphate, Tribasic, 375, (S3)54 Sodium Phosphate TS, 855 Sodium Polyphosphate, Insoluble Sodium Polyphosphates, Glassy, 375, (S2)31, (S3)55 Sodium Potassium Tartrate, 376 Sodium Potassium Tripolyphosphate, 377, (S3)56 Sodium Propionate, 377 Sodium Pyrophosphate, 378 Sodium Pyrosulfite, 369 Sodium Saccharin, 378 Sodium Sesquicarbonate, 380 Sodium Silicoaluminate, 351 Sodium Stearoyl Lactylate,380 Sodium Stearyl Fumarate, 382 Sodium Sulfate, 383 Sodium Sulfide TS, 855 Sodium Sulfite, 383
138 / Cumulative Index
Sodium Sulfite, Exsiccated, 383 Sodium Tartrate, 384 Sodium Tetraphenylborate TS, (S2)45 Sodium Tetrapolyphosphate, 375, (S2)31, (S3)55 Sodium Thiosulfate, 384 Sodium Thiosulfate, 0.1 N, 859 Sodium Thiosulfate TS, 855 Sodium Trimetaphosphate, 385, (S3)56 Sodium Triphosphate, 385, (S1)41, (S3)57 Sodium Tripolyphosphate, 385, (S1)41, (S3)57 Softening Point, 727, 832 Drop Method, 832 Ring-and-Ball Method, 834 Solidification Point, 728, 742 Solin Oil, (S3)58 Solubility in Alcohol, 449, 819 Solubility (Table), 7 Soluble Saccharin, 378 Solutions, Colorimetric (CS), 848 Solutions, Standard, for the Preparation of Controls and Standards, 849 Solutions, Standard Buffer, 848 Solutions, Test (TS) and Other Reagents, 5, 849 Solutions, Volumetric, 855 Solutions and Indicators, 5, 848, 860, (S1)114, 116, (S3)110 Sorbic Acid, 387, (S3)59 Sorbitan, Monododecanoate, 306 Sorbitan, Monooctadecanoate, 307 Sorbitan, Mono-9-octadecenoate, 308 Sorbitan Monostearate, 387 D-Sorbite, 388, (S2)32 Sorbitol, 388, (S2)32 D-Sorbitol, 388, (S2)32 Sorbitol Solution, 389 Soybean Oil (Unhydrogenated), 390 Soy Protein Concentrate, (S3)59 Spearmint Oil, 391, 600 Specifications, Procedure for Revising, xxii Specifications, Procedures for Submission and Development of, xxi Specifications for Flavor Chemicals, 449 Specific Gravity, 5, 449 Specific Gravity (Fats and Related Substances), 827 “Specificity,” Defined, xxiv Specific Rotation, 739 Spice Oleoresins, 391, (S1)42 Angelica Seed, 391, 392 Anise, 391, 392 Basil, 391, 392 Black Pepper, 391, 392 Capsicum, 391, 392 Caraway, 392 Cardamom, 392
FCC IV, Supplement 3
Celery, 392 Coriander, 392 Cubeb, 392, 393 Cumin, 392, 393 Dillseed, 392, 393 Fennel, 392, 393 Ginger, 392, 393 Hop, 392, 393 Laurel Leaf, 392, 393 Marjoram Sweet, 392, 393 Origanum, 392, 393 Paprika, 392, 393 Parsley Leaf, 392, 393 Parsley Seed, 392, 393 Pimenta Berries, 392, 393 Rosemary, (S1)43 Thyme, 392, 393 Turmeric, 392, 393 Spike Lavender Oil, 393, 594 Stability (Active Oxygen Method), 828 Standard Ammonium Solution, 849 Standard Barium Solution, 849 Standard Buffer Solutions, 848 Standard Iron Solution, 849 Standard Magnesium Solution, 849 Standard Phosphate Solution, 849 Standard Solutions for the Preparation of Controls and Standards, 849 Stannous Chloride, 394 Stannous Chloride TS, 855 Starch, Acid-Modified, 159 Starch, Bleached, 159 Starch, Gelatinized, 159 Starch, Hydroxypropyl, 160 Starch, Oxidized, 159 Starch, Thin-Boiling, 159 Starch Acetate, 159 Starch Aluminum Octenyl Succinate, 160 Starch Esters, 159 Starch Ether–Esters, 159 Starch Ethers–Hemiacetals, or Ethers, 159 Starch Iodate Paper, 862 Starch Iodide Paper, 862 Starch Iodide Paste TS, 855 Starch Octenyl Succinate, 159 Starch Phosphate, 159 Starch Sodium Octenyl Succinate, 159 Starch Sodium Succinate, 169 Starch TS, 855 Starter Distillate, 394 Stearic Acid, 395 Stearin, 185 Stearyl Monoglyceridyl Citrate, 396 Sterculia Gum, 208 Strawberry Aldehyde, 492 Strong Ammonia Solution, 26 Stronger Ammonia TS, 850 Stronger Ammonia Water, 26, 850 Styrene, Bound, 782
Styrene, Residual, 784 Submission and Development of Specifications, Procedures for, xxi Submissions to the Codex, xxii Succinic Acid, 397 Succinylated Monoglycerides, 397 Sucralose, 398, (S2)33 Sucrose, 400, 846, (S2)35 Sucrose Acetate Isobutyrate, (S3)60, 101 Sucrose Fatty Acid Esters, (S1)44 Sucroesters, (S1)44 Sugar, 400, (S2)35 Sugar Beet Fiber, (S1)45 Sugar Beet Pulp, (S1)45 Sulfanilic Acid TS, 855 Sulfate and Chloride Limit Test, 757 Sulfate Identification Test, 755 Sulfite Identification Test, 755 Sulfur (by Oxidative Microcoulometry), 780 Sulfur Dioxide, 401 Sulfur Dioxide Detector Tube, 862 Sulfur Dioxide Determination, 841 Sulfur Dioxide Policy, 2 Sulfuric Acid, 402, 855 Sulfuric Acid (reagent), 855 Sulfuric Acid, 1 N, 859 Sulfuric Acid, 95%, 855 Sulfuric Acid, Alcoholic, 0.5 N, 859 Sulfuric Acid, Alcoholic, 5 N, 859 Sulfuric Acid Table, 752 Sulfuric Acid TS, 855 Sulfuric Acid TS, Diluted, 855 Sulfurol, 524, (S3)84 Summer Savory Oil, 346 Sunflower Oil (Unhydrogenated), 403 Sunset Yellow FCF, 146, (S3)29 Superglycerinated Fully Hydrogenated Rapeseed Oil, 337, (S3)45 Sweet Basil Oil, 39 Sweet Orange Oil, 273 Sweetwood Bark Oil, 91 Synthetic Amorphous Silica, 348, (S3)51 Synthetic Magnesium Silicate, 235 Synthetic Paraffin, Oil Content of, 750 Synthetic Terpene Resin, (S2)37 Synthetic Wax, 291
T Talc, 404 Tallow, 405 Tangerine Oil, Coldpressed, 405, 595 Tangerine Oil, Expressed, 405 Tannic Acid, 406 Tannic Acid TS, 855 Tared Container, 6 Tarragon Oil, 407, 595 Tartaric Acid, 407
FCC IV, Supplement 3
L(+)-Tartaric Acid, 407 Tartrate Identification Test, 755 Tartrazine, 145, (S3)28 TBHQ, 408 Temperatures, 5 Terpene Resin, Natural, 410, (S2)36 Terpene Resin, Synthetic, 410, (S2)37 ␣-Terpinene, 554 ␥-Terpinene, 554 Terpinen-4-ol, 554, (S3)88 ␣-Terpineol, 554, 710, (S1)100, (S3)88 Terpinyl Acetate, 556, 676, (S1)100, (S3)88 Terpinyl Propionate, 556, 711, (S1)100, (S3)88 Test Methods for Flavor Chemicals, 449, 564, (S1)106, (S1)116 Acidity Determination by Iodometric Method, 565 Acid Value, 568, 815 Alcohol Content of Ethyl Oxyhydrate, 565 Aldehydes—Hydroxylamine Method, 564, (S1)116 Aldehydes—Hydroxylamine/Tert-Butyl Alcohol Method, 564 Assay by Gas Chromatography, 564 Assay by Titrimetric Procedures, 565 Assays for Certain Aldehydes and Ketones, 564 Direct Aqueous Acid–Base Titrations, 565 Direct Aqueous–Alcoholic Acid–Base Titrations, 565 General Method, Nonpolar Method, 564 General Method, Polar Method, 564 Ketones—Hydroxylamine Method, 565, (S1)116 Limit Test for Antioxidants in Ethyl Acrylate, 566 Limit Test for Heavy Metals, 567 Limit Test for Hydrocarbons in Eugenol, 567 Limit Test for Hydrocyanic Acid in Benzaldehyde, 567 Limit Test for Lead, 567 Limit Test for Methyl Compounds in Ethyl Acetate, 567 Limit Test for Peroxide Value, 567 Limit Test for Readily Carbonizable Substances in Ethyl Acetate, 567 Limit Test for Readily Oxidizable Substances in dl-Menthol, 567 Limit Test for Reducing Substances, 568 Procedure Requiring the Use of Sealed Glass Vials or Ampules, 564, (S1)116 Qualitative Test for Phenols Using Ferric Chloride, 568
Cumulative Index / 139
Residue on Evaporation, 568 Test Solutions (TS) and Other Reagents, 5, 849 Tetrabromo-m-cresolsulfonphthalein, 860 Tetrabromophenolsulfonphthalein, 860 Tetradecanal, 534 Tetradecanoic Acid, 262 1-Tetradecanol, 536 Tetradecyl Alcohol, 536 Tetrahydrofurfuryl Alcohol, 556, 640 Tetrahydrogeraniol, 482 Tetrahydrolinalool, 556 Tetrahydro-2H-1,4-oxazine, 261 2,3,5,6-Tetramethylpyrazine, 556, 641 Tetrapotassium Pyrophosphate, 326, (S3)41 Tetrasodium Diphosphate, 378 Tetrasodium Pyrophosphate, 378 Thermometers, 727 Thiamine Chloride, 411 Thiamine Hydrochloride, 411 Thiamine Mononitrate, 412 Thiamine Nitrate, 412 Thiamin Hydrochloride, 411 Thiamin Mononitrate, 412 Thibetolide, (S1)56 Thin-Boiling Starch, 159 Thin-Layer Chromatography, 731 Thiobismethane, 482, (S3)70 Thiosulfate Identification Test, 755 Thorium Nitrate, 0.1 M, 859 L-Threonine, 413, (S3)60 Thuja Oil, 94 Thyme Oil, 413, 595 Thyme Oleoresin, 392, 393 Thymol, 556, 641, (S1)100 Thymol Blue, 861 Thymol Blue TS, 851, 855 Thymolphthalein, 861 Thymolphthalein TS, 855 Thymolsulfonphthalein, 861 Tight Container, 7 Time Limits, 6 Titanium Dioxide, 414 DL-␣-Tocopherol, 417, (S2)37 D-␣-Tocopherol Concentrate, 418 Tocopherols Concentrate, Mixed, 419 D-␣-Tocopheryl Acetate, 420 DL-␣-Tocopheryl Acetate, 421, (S1)115 D-␣-Tocopheryl Acetate Concentrate, 422 D-α-Tocopheryl Acetate Preparation, 422 D-␣-Tocopheryl Acid Succinate, 422 Tolerances, 6 Tolualdehyde, 558, (S1)102 p-Tolualdehyde, 558 Toluene Distillation Method for Water, 747 α-Toluic Acid, 546
α-Toluic Aldehyde, 546 p-Tolyl Acetate, 474 Tolyl Acetate, So-Called, 526 p-Tolyl Aldehyde, 558 Tolyl Aldehyde, mixed isomers, 558 p-Tolyl Isobutyrate, 558, 641, (S1)102 Torula Yeast, 440 Total Alcohols, 815 Total Ash, 748 Total Color, 773, 774 Total Monoglycerides, 824 Total Solids, 842 Glucose Syrup (Corn Syrup), 843, 843 High-Fructose Corn Syrup Solids, 844 Maltodextrin, 845 Sucrose, 846 Total Unsaturation, 785, (S2)42 Trace Impurities, xx, 6 Tragacanth, 424 “Transfer,” Defined, 4 Triacetin, 424, (S3)61 Triatomic Oxygen, 277 Tribasic Magnesium Phosphate, (S2)15 Tribasic Potassium Phosphate, (S2)28, (S3)41 Tribasic Sodium Phosphate, (S3)54 Tributyrin, 558, 677, (S1)102 Tricalcium Phosphate, 69, (S1)10 Trichloroethene, 425 Trichloroethylene, 425 1,1,2-Trichloroethylene, 425 4,1',6'-Trichlorogalactosucrose, 398, (S2)33 2-Tridecenal, 558, 642, (S1)102, (S3)88 Triethanolamine, 0.5 N, 860 Triethyl Citrate, 426 3,7,12-Trihydroxycholanic Acid, 99 Triketohydrindene Hydrate TS, 853, 855 Trimagnesium Phosphate, 234, (S2)15 Trimethylamine, 558, (S3)88 4-Trimethylamino-3-hydroxybutyrate, (S2)5 2,6,6-Trimethylbicyclo[3.1.1]hept-2-ene, 550, (S3)86 4(2,6,6-Trimethyl-1-cyclohexenyl)-3butene-2-one, 510 4(2,6,6-Trimethyl-2-cyclohexenyl)-3butene-2-one, 510 3,7,11-Trimethyl-1,6,10-dodecatrien-3-ol, 536, (S3)84 3,7,11-Trimethyl-2,6,10-dodecatrien-1-ol, 498, (S3)74 3,5,5-Trimethyl Hexanal, 558, (S3)88 2,4,5-Trimethyl ␦-3-Oxazoline, 560, 677 2,3,5-Trimethylpyrazine, 560, 642, (S1)102, (S3)90 1,3,7-Trimethylxanthine, 52 Trinitrophenol TS, 854, 855 Triphosphate, 385, (S1)41, (S3)57
140 / Cumulative Index
Tripotassium Phosphate, 325, (S2)28, (S3)41 Tripropionin, 500 Trisodium Dipotassium Tripolyphosphate, 377, (S3)56 Trisodium Phosphate, 375, (S3)54 Tristearin, 185 Tropaeolin D, 861 Trypsin, 133, 788, (S3)18 Trypsin Activity, 814 DL-Tryptophan, 426 L-Tryptophan, 427 Tunu, 249 Turmeric Oleoresin, 392, 393 L-Tyrosine, 427
U Ultraviolet Absorbance of Citrus Oils, 819 ␦-Undecalactone, 560, 642, (S1)104 ␥-Undecalactone, 560, 642, (S1)104 Undecanal, 560, 677 2-Undecanone, 560, 643 1,3,5-Undecatriene, (S1)56, (S3)90 10-Undecenal, 560, 643 Undecen-10-al, 560 2-Undecenol, 560, 678 (E)-2-Undecenol, (S1)104, (S3)90 trans-2-Undecenol, (S1)104, (S3)90 Undecyl Alcohol, 562, 678 n-Undecyl Aldehyde, 560 Unsaponifiable Matter, 828 Urea, 428
V “Vacuum,” Defined, 6 Valeraldehyde, 562, 564, 643 Valeric Acid, 562, 565, 678, (S1)104 ␥-Valerolactone, 562, 679 “Validation,” Defined, xxiii Validation of Codex Methods, xxii L-Valine, 429, (S3)62 Vanillin, 562, 679 Venezuelan Chicle, 249
FCC IV, Supplement 3
Veratraldehyde, (S1)56, (S3)90 Veratryl Aldehyde, (S1) 56, (S3)90 1-Vinyl-2-pyrrolidone Crosslinked Insoluble Polymer, 309 Viscosity, 743, (S1)109 Viscosity (Rosins and Related Substances), 835 Viscosity of Cellulose Gum, (S1)111, (S2)48 Viscosity of Dimethylpolysiloxane, 743, (S1)110 Viscosity of Methylcellulose, 743, (S1)111 Viscosity of Sodium Carboxymethylcellulose, 744 Vital Wheat Gluten, 535 Vitamin A, 429 Vitamin B1, 411, 412 Vitamin B1 Hydrochloride, 411 Vitamin B1 Mononitrate, 412 Vitamin B2, 338 Vitamin B6, 334 Vitamin B6 Hydrochloride, 336 Vitamin B12, 431 Vitamin C, 33 Vitamin C Sodium, 354 Vitamin D, 432, 434 Vitamin D2, 432 Vitamin D3, 434 Vitamin K, (S1)47 Volatile Acidity, 829 Volatile Oil Content (Essential Oils and Flavors), 815 Volatile Oil Content (Oleoresins), 832 Volumetric Apparatus, 4, 728 Volumetric Solutions, 855 “VS,” Defined, 449
W Water and Loss on Drying, 4, 6, 749 Water Determination, 745 Karl Fischer Titrimetric Method, 745 Toluene Distillation Method, 747 Water Vapor Detector Tube, 862
Weighing Practices, 6 Weights and Balances, 4, 729 Weights and Measures, Symbols, and Abbreviations, 6 Well-Closed Container, 7 Wheat Gluten, 435 Whey, 435, (S1)48 Whey Protein Concentrate, (S1)51 Whey, Reduced Lactose, (S1)50 Whey, Reduced Minerals, (S1)51 White Cedar Leaf Oil, 94 White Petrolatum, 289 White Shellac, 347 White Wax, 40 Wine Yeast Oil, 108 Wintergreen Oil, 437, 600 Wool Fat, 216, (S3)31
X Xanthan Gum, 437 Xylenol Orange, 861 Xylenol Orange TS, 855 Xylitol, 439, (S2)38
Y Yam Flour, 210, (S1)27 Yeast, Autolyzed, (S1)52 Yeast, Dried, 440 Yeast Extract, 442, (S1)53 Yellow Petrolatum, 289 Yellow Prussiate of Soda, 363 Yellow Wax, 41
Z Zein, 443 Zinc Gluconate, 443 Zinc Identification Test, 755 Zinc Oxide, 445, (S1)116 Zinc Sulfate, 445 Zinc Sulfate, 0.05 M, 860 Zingerone, 562, (S3)90