Food Analysis Third EditionFOOD SCIENCE TEXT SERIES: ‘The Food Science Text Series provides faculty with the leading teaching tools. The Editorial Board has outlined the most appropriate and complete content for each food science course in a typical food science program, and has identified textbooks of the highest quality, written by leading food science educators, EDITORIAL BOARD Series Editor Dennis R. Heldman, Professor of Food Engineering, Department of Food Science and Director of Cooperative Research & Development Program, Center for Advanced Food Technology, Rutgers, The State University of New Jersey. Board Members Richard W. Hartel, Professor of Food Engineering, Department of Food Science, University ‘of Wisconsin, Hildegarde Heymann, Professor of Sensory Science, Department of Food Science & Technology, University of California—~Davis Joseph H. Hotchkige, Professor, Institute of Food Science and Institute for Comparative and Environmental Toxicology, and Chair, Food Science Department, Cornell University, James M. Jay, Professor Emeritus, Department of Nutrition and Food Stience, Wayne State University and Adjunct Professor, University of Nevada—-Las Vegas. Kenneth Lee, Professor and Chair, Department of Food Science and Technology, The Ohio State University. Norman G. Marriott, Emeritus Professor & Extension Food Scientist, Department of Rood ‘Science and Technology, Virginia Polytechnic and State University: Joseph Montecalvo, Jr.. Professor, Department of Food Science and Nutrition, California Polytechnic and State University—San Luis Obispe. 5, Suzanne Nielsen, (rofessor of Food Science, Department of Food Science, Purdue University J. Antonio Toes, Associate Professor of Food Science, Department of Food Science and Technology, Oregan State University Titles Elementary Food Science, Fourth Edition, Emest R. Vieira (1996) Essentiale of Food Sanitation, Norman G, Marriott (1997) Fusentials of Food Science, Second Edition, Vickie A. Vaclavik and Elizabeth W Christian 2003) Food Analysis, Third Edition, S. Suzanne Nielsen (2000) Food Analysis Laboratory Manual, S, Suzanne Nielsen (2003) Food Science, Fifth Edition, Norman N. Potter and Joseph H. Hotchkiss (1995) Fundamentals of Food Process Engineering, Second Edition, Romeo T- Toledo (1990) Introduction to Food Process Engineering, P. G. Smith (2003) Modern Food Microbiology, Sixth Edition, James M. fay (2000) Principles of Food Chemistry, Third Edition. John M. deMan (1999) Principles of Food Processing, Dennis R. Heldman and Richard W. Hactel (1997) Principles of Food Sanitation, Fourth Edition, Norman G. Marriott 1999) ‘Sensory Evaluation of Food: Principles and Practices, Harry T. Lawless and Hildegarde Heymann (1998)Food Analysis Third Edition edited by S. Suzanne Nielsen Purdue University West Lafayette, Indiana KLUWER ACADEMIC/PLENUM PUBLISHERS New York @ Boston ¢ Dordrecht @ London # MoscowLibary of Congress Cataloging: in- Publication Dasa Food analysis/edited by 8. Suzanne Nielson, 3rd ed Poco Includes bibliographical references aed index TSBN 0:306-47495-6 L. Food—Analysis, 1. Nielsen, 8. Suan. "TBA P54 200 68! 7 deal o0R0664 ISHN: OsOU7EER 2000 Kluwer Avacimie (Plenum Publishers, New York 253 Spring Street, New York, Newe York 1015, itpiffiowcwap com Wosrasaaa ACUTE: read for this book is avaiable frm the I ibrany of Congas Alt sights served ‘No pate of this Book may be reproduced, starve in a retsicwalsystorn, or transmitted 4 any form af lay any moons, electri, mechanical, photocupyin'g, microfilming, recording, or ateewise, without ‘written permission from the Publisher, with the exception of any matecial supplied specifically for the purpose of being entered and executed on 2 computer system, For exclusive Use by the purchaser of he work, Permissions for bucks published in Forage: permissions af Vormfasions tor books published in the United States of Amevica: rinissionsutap ce Printed in the United States of AmetisaContents Contributing Auinors vii Preface and Ackiiweledgments ix List of Abbreviations vi Part, General information 1. Introduction to Food Analysis 3 S. Suzame Nielsen 2. United Statos Government Regulations and International Standards Related to Food Analysis 15 5. Suzamie Nioksen 3. Nutrition Labeling 35 S$. Suzminie Nielsen snd Lloyd E. Metzger 4. Bvaluation of Analytical Data St |. Scott Smt Sampling and Sample Preparation 65 Andrew Proctor and fonn-Frimigais Meultenet Part ll. Compositional Analysis of Foods 6 Moisture and Total Solids Analysis 81 Robert L. Bradley, fr. 7. Ash Analysis 103 Loniel H. Harbers and 8, Suzanne Nielsere 8. Crude Fat Analysis 113 David B, Min and Jeff M4. Boff 9. Protein Analysis 131 Sain KC. Chang 10, Carbohydrate Analysis 143 Jamies N, BeMitler Mu. 12, 16. VW. 18, 19. 20. Vitamin Analysis 175 Ronald R. Eitewmiler and W.O. Landen, Jr. Mineral Analysis 189 Charles E. Carpenter and Deloy G. Hendricks Chemleal Properties and Characteristics of Foods pHand Titratable Acidity 207 George D. Sailer and Patrict A. Murphy Fat Characterization 227 Oscar A. Pike Protein Separation and Characterization Procedures 247 Denise M. Smiths Application of Enzymes in Food Analysis 269 Joseph R. Powers Immunoassays 287 Peter Sporns Agricultural Biotechnology (GMO} Methods of Analysis 302 Anure R. Bridges, Kimberly M. Magirr, and Janes W Stave Analysis of Pesticide, Mycotoxin, and Drug Residues in Foods 318 William D. Marshall Analysis for Extraneous Matter 341 John R. Pedersen Determination of Oxygen Demand 351 Youg D. Hangvi Contents PartlV. Spectroscopy 22. Basic Principles of Spectroscopy 359 ‘Michael H. Penner 23. Ultraviolet, Visible, and Fluorescence Spectroscopy 371 Michael H, Penner 24, Infrared Spectroscopy 387 Randy L. Wehling 25. Atomic Absorption and Emission Spectroscopy 401 Dennis D. Miller and Michael A. Rutzke 26, Mass Spectrometry 423 I. Scott Smith and Rohan A. Thakur PartV. Chromatography 27. Basic Principles of Chromatography 437 ‘Mary Ann Rounds and 8, Suzanne Nielsen 28. High Performance Liquid Chromatography 461 Mary Arm Rounds and Jesse F. Gregory, IHL 29, Gas Chromatography 479 Gary A. Reineccius 7 PartVi. Physical Properties of Foods + 30. Rheological Principles for Food Analysis 503 Christopher R. Dautert and E. Allen Foegeding 3k Thermal Analysis 517 Timothy W. Schenz 32, Color Analysis 529 F Jack Francis Index 543,Contributing Authors James N. BeMiller Department of Food Science Purdue University West Lafayette, Indiana 47907-1160 Jeff M. Boff Department of Food Science and Technology ‘The Ohio State University Columbus, Olnio 43210 Robert L. Bradley, Jr. retired!) Formerly, Department of Food Science University of Wisconsin Madison, Wisconsin 53706 Anne R. Bridges Medallion Laboratories General Mills Minneapolis, Minnesota 55427 Charles E. Carpenter Department of Nutrition and Food Sciences Utah State University Logan, Utah 84322-8700 Sam K.C. Chang Department of Cereal and Food Sciences North Dakota State University Fargo, North Dakota $8105 Christopher R. Daubert Department of Food Science North Carolina State University Raleigh, North Carolina 27695-7624 Ronald R. Fitenmiller Department of Food Science University of Georgia Athens, Georgia 30602 E, Allen Foegeding Department of Food Science North Carolina State University Releigh, North Carolina 27695-7624 F Jack Francis (retired) Formerly, Department of Food Science University of Massachusetts Amherst, Massachusetts (1003 Jesse F Gregory, Ill Department of Food Science and Human Nutrition University of Florida Gainesville, Plorida 32611-0970 Yong D. Hang Department of Food Science and Technology Cornell University Geneva, New York 14456 Leniel H. Harbers (retired) Formerly, Department of Animal Sciences and Industry Kansas State University Manhattan, Kansas 66506-1600 Deloy G. Hendricks Department of Nutrition and Food Sciences Utah State University Logan, Utah 84322-4700 W. 0. Landen, Jr Department of Food Science University of Georgia Athens, Georgia 30601 Kimberly M. Magin Monsanto Co. St. Louis, Missouri 63198 William D. Marshall Department of Food Science and Agricultural Chemistry MacDonald Campus of McGill University St-Anne-de-Bellevuc, Quebec H9X 3V9 Canada Lloyd £. Metzger Department of Fuod Science and Nutrition University of Minnesota $1. Paul, Minnesota 55208-6099 Jean-Francois Meullenet Department of Food Science University of Arkansas Fayetteville, Arkansas 72703 vilvilt Convituting Authors Dennis D. Miller Department of Food Science Cornell University Ithaca, New York 14853-7201 David B. Min Department of Food Science and Technology ‘The Ohio State University Columbus, Ohio 43210 Patricia A. Murphy ‘Department of Food Science and Human Nutrition Jowa State University ‘Ames, Iowa 50071 S. Suzanne Nielsen Department of Food Science Purdue University West Lafayette, Indiana 47907-1160 John R. Pedersen (retired) Formerly, Department of Grain Science and Industry Kansas State University Manhattan, Kansas 66506-2201 ‘Michael H. Penner Department of Food Science and Technology Oregon State University Corvallis, Oregon 97331-6602 Oscar A. Pike Department of Nutrition, Dieteties, and Food Science Brigham Young University Provo, Utah 84602 Joseph R. Powers Department of Food Science and Human Nutrition Washington State University Pullman, Washington 99164-5184 Andrew Proctor Department of Food Science University of Arkansas Fayetteville, Arkansas 72703 Gary A. Reinecciuss Departtnent of Food Science and Nutrition University of Minnesota St. Paul, Minnesota 55108-6099 Mary Ann Rounds (deceased) Department of Physics Purdue University ‘West Lafayette, Indiana 47907 Michael A. Rutzke US. Plant, Soil, and Nutrition Laboratory USDA/ARS. Comell University Ithaca, NY 14853 © George D. Sadler National Center for Food Safety and Technology Mlinois Institute of Technology Summit-Argo, Ilinois 60501 Timothy W. Schenz. Abbott Laboratories Ross Products Division Columbus, Ohio 43216 Denise M. Smith Department of Food Science and Toxicology University of Idaho Moscow, [daho 83844-2201 J. Scott Smith Department of Animal Sciences and Industry Kansas State University Manhattan, Kansas 66506-1600 Peter Sporns Department of Agriculture, Food & Nutritional Science University of Alberta Edmonton, Alberta T6G2P5 Canada James W. Stave ‘Strategic Diagnostics Inc. Newark, Deleware 19713, Rohan A. Thakur Finnigan Corporation: A Thermo Quest Company San Jose, California 95134-1991 Randy L. Wehling Department of Food Science and Technology University of Nebraska Lincoln, Nebraska 68583-0919Preface and Acknowledgments The intent of this book is the same as that described in the Preface to the first and second editions—a text primarily for undergraduate students majoring irefood science, currently studying the analysis of foods. How- ever, comunents from users of the first and second editions have convinced me that the book is also valu- able text for persons in the food industry who either do food analysis or interact with analysts, ‘The following summarizes changes from the sec- ond edition: (1) Reorganized chapter order and group- ing in the middle section of the book, (2) Com- ined scloct chapters (eg, fiber analysis combined with carbohydrate analysis; protein nutritional quality condensed and moved into chapter on protein sep- aration and characterization}, (3) Condensed select chapters (eg, government regulations), (4) Changed immunoassay chapter to focus primarily on enzyme: Yinked immunosorbent assays, (5) Added chapter on agricultural biotechnology (GMO) methods of analy- sis, (6) Updated all chapters as appropriate to delete little used techniques and add new methods, and (7) Deleted some chapters not widely used in teaching an undergraduate course in food analysis. Regrettably, in an effort to make the book a more manageable size and cost, especially for students, two excellent chapters of advanced techniques from the second edition (ie., magnetic resonance and analysis of food emulsions) are not included in the third edi- tion, Readers who need that information are referred to those chaptersin the second edition and also to detailed ‘books on those techniques. Also, the requests by some users of this book to add chapters on other topics (e.g., HACCP, sensory evaluation) were considered carefully. However, restrictions on size and cost of the textbook, and the availability of other resources on these topics, have prevented their inclusion in this book. ‘As stated for the first and second editions, the chapters in this texibook are not intended as detailed references, but as general introductions to the top- ics and the techniques. Course instructors may wish to provide more details on a particular topic to stu- dents. Chapters focus on principles and applications of techniques. Procedures given are meant to help explain the principles and give some examples, but are not ‘meant to be presented in the detail adequate to actually conduct a specific analysis. As in the first and sec- ond editions, all chapters have summaries and study questions, and key words or phrases are in bold type, tohelp students focus their studies. In this third edition, the middle section of the text has been rearranged into a group of chapters on compositional analysis and one on chemical properties and characterization, Hopefully {instructors will find this arrangement an improvement, but instructors are encouraged to cover the topics from this text in whatever order is most suitable for theit course. In preparing this third edition, the new compe- tency requirements established by the Institute of Food ‘Technologists were considered. Those requirements relevant to food analysis are as follows: (1) Under standing the principles behind analytical techniques associated with food, (2) Being able to select the appropriate analytical technique when presented with a practical problem, and (3) Demonstrating practical Proficiency in food analysis laboratory. This textbook should enable instructors to meet the requirements and develop learning objectives relevant to the first two of these requirements, The laboratory manual devel- ‘oped to accompany this third edition should bea useful resource to help students meet the third requirement. Tam grateful to first-, second-, and thitd-time chapter authors for agreeing to be a part of this project. Many authors have drawn on their experience of teach ing students and /or experience with these analyses to give chapters the appropriate content, relevance, and ease of use. | also want to thank the "resource per- sons” from the food industry who help the students, inthe food analysis courses [teach each year, ona spe- al project I assign related to quality assurance. These projects area constant guide to me in determining what methods to include in this text. I wish to thank the authors of articles and books, and well as the publish: ers and industrial companies, for their permission to reproduce materials used here. Ivery much appreciate the valuable suggestions and contribution of new study ‘questions for this 3rd edition made by Dr Lloyd Met- zger of the University of Minnesota. Special thanks is extended to Erin Addison, Susan Axe! Bedsaul, Joanne DeRoeck, Wilfredo Dominguez, Christina Kokini, and. Cynthia Machado at Purdue University for their assis- tance in word processing, editing, and checking details in the preparation of this book. S. Suzanne NielsenList of Abbreviations AACC AAS ARTS AC ADP AES AMS ANS AOAC Aocs AOM APCI APHA, APPT ASE, ASTM ATCC ATE ATP. ATR ATR-FTIR, BAW BCA BCR Be BHA BHT BOD. BSA BSDA Bt CAST cD coc ct CRIA CER GMP a cE cD cD American Association of Cereal Chemists atomic absorption spectroscopy 222-arino-di-3-ethylbenzthiazoline-6- sulfonate alternating current adenosine-S'-diphosphate atomic emission spectroscopy Agticultural Marketing Service ‘Lranilino & naphthalene sulfonic acid Association of Official Analytical Chemists American Oil Chemists’ Society active oxygen method atmospheric pressure chemical ionization American Public Health Association atmospheric pressure phote-ionization accelerated solvent extraction American Society for Testing Materials American Type Culture Collection Bureau of Alcohol, Tobacco, Firearms and Explosives adenasine-5'-triphosphate attenuated total reflectance attenuated total reflection-Fourier transform infrared ‘base and acid washed bicinchoninic acid Community Bureau of Reference Baumé modulus ‘butylated hydroxyanisole butylated hydroxytoluene biochemical oxygen demand ‘bovine serum albumin Baciltus stearothermophitis disk assay Bacilus thuringiensis calf antibiotic and sulfa test charge-coupled device Centers for Disease Control commercial factor Canadian Foad-Inspection Agency Code of Federal Regulations (Current Good Manufacturing Practices chemical ionization confidence interval charge injection device Commercial Item Description cE CLND cmc CNBr cop Qc wv cv DAL DE DEA DEAT DFE DHHS DMD DMSO DMTA DNEB DNP. pr DRV DSHEA, DTA DINB dw EAAL EBT ECD EDS EDTA EEC £1 HIE ELCD ELISA EPA ERH ESA. ESI ETO ‘Commission Internationale d'Eclairage chemiluminscent nitrogen detector critical micelle concentration cyanogen bromide chemical oxygen demand 2,6-dichloroquinonechloroimide coefficient of variation Center for Veterinary Medicine defect action level dizect current degree of esterification dielectric analysis dielectric thermal analysis, dietary folate equivalent Department of Health and Human Services malate dehydrogenase dimethyl sulfoxide dynamic mechanical thermal analysis, I-fluoto-2,4-dinitrubenzene dinitrophenyl deoxynivalenol degree of polymerization Daily Reference Value differential scanning calorimetry Dietary Supplement Health and Education Act differential thermal analysis 5,8'-thiobis-2-nitrobenzoic acid difforential thermal rheometry daily value dry weight basis essential amino acid index. eriochrome black T electron capture detector energy dispersive spectroscopy ethylenediaminetetraacetic acid European Economic Community electron impact easily ionized elements electrolytic conductivity detector enzyme linked immunosorbent assay Environmental Protection Agency equivalents equilibrium relative humidity electrokinetic sonic amplitude electrospray interface ethylene oxidexii List ob Aburestaions. FAME FAO/WHO FAS ee FDA FDAMA FD&C FDNB FRA HID FIFRA FNB/NAS: FD FQPA FSIS FT Frc FEICR FTIR GATT ica GC-AED CCETIR GCMs GEC airs GLC CMA CMO, GMP corop crc G6PDH HACCP, HETP ‘HFS HK HPLC HPLC-MS: HPTLC HRGC iP ICP-AES ICTA 1D fatty acid methyl esters Food and Agricultural Organization/ World Health Organization ferrous ammonitim sulfate Food Chemicals Codex Food and Drug Administration Foods and Drug Administration. Modernization Act Food, Drug and Cosmetic L-fluaro-2,4-dinitrobenzene free fatty acid flame tonization detector Federal Insecticide, Fungicide, and Radenticide Act Food and Nutrition Board of the National Academy of Sciences flame photometric detector Food Quality Protection Act Food Safety and Inspection Service Rourier transform Fedetal Trade Commission Fourier transform-ion cyclotron Fourier transform infrared General Agreement on Tariffs and Trade gas chromatography {gas chromatogeaphy-atomiic emission detector gas cheomatogeaphy-Fourier transfor infrared gas chromatography-mass spectrometry gel filtratinn chromatography Grain Inspection, Packers and Stockyard Administration gas-liquid chromatography Grocery Manufacturers of America genetically modified organism Good Manufacturing Practices glucose oxidase/ peroxidase gel-permeation chromatography sglacose-6-phosphate dehydrogenase Hazard Analysis Critical Control Point height equivalent to a theoretical plate high fractose syrup hexokinase high performance liquid chromatography high performance liquid chromatography-mass spectroscopy high performance thin-layer chromatography high resolution gas chromatography inductively coupled plasma inductively coupled plasma-atomic emission spectroscopy International Confederation for Thermal Analysis inner diameter IDK Igk. IgG. IMS InGaAs INT fava IR IRMM Ss ISA ISE 150 wu JUPAC JECEA keal KER KFRog Kup LALLS. Le LC-MS LFS LMS Ls MALDLTOF MCL Mpes'* mEq ‘MeSCN MLR MRMs MS MS/MS Ms" MW jz NAD NADP NADPH NCWM NEDM NIR NIST NLEA insect damaged kernels immunoglobulin E immunoglobulin G Interstate Milk Shippers indium-gallium-arsenide indonitrotetrazolium Integrated pest management infrared Institute for Reference Materials and ‘Measurements internal standard ionic strength adjustor ion-selective electrode International Organization for Standardization International Units International Union of Pure and Applied Chemistry Joint FAO/WHO Expert Committee on Food Additives kilo-calorie Karl Fischer reagent Karl Fischer reagent water equivalence potassium acid phthalate Jow-angle laser light scattering liquid chromatography liquid chromatography-mass spectroscopy lateral flow strip laboratory information management system labeled serving matrix-assisted Inser desorption time-of-flight maximum contaminant level modulated differential scanning, calorimeter! milliequivalents methylthivcyanate multiple linear regression multiresidue methods mass spectrometry (or spectrometer) tandem MS, multiple stages of mass spectrometry molecular weight -mass-to-charge ratio nicotinarnide-adenine dinucleotide nicotinamide-adenine dinucleotide phosphate reduced NADP National Conference on Weights and Measures non fat dry milk near-infrared Nationat Institute of Standards and Technology Nutrition Labeling and Education ActList of Abbreviations lif NMFS NMR NOAA NPD NRC NSSP od op ODS OFS OPA OPs O81 PAD PACE PAM! PAM IL PCBs PCR PCR PDC PDCAAS pat PEEK PER pl Pip PLs PMO eMT ppb PPD. ppm ppt PieGin PTFE PUFA PVPP RA Rac RCS RDI Ry RF RD RGB RI RIA ROSA RPAR RVA rpm SAsO National Marine Fisheries Service nuclear magnetic resonance National Oceanic and Atmospheric Administration nitrogen phosphorus detector or thermionic detector National Research Council National Shellfish Sanitation Program organochlorines outer diameter octadecylsily! optical emission spectroscopy o-phthalaldehyde organophosphates oil stability index pulsed-amperometric detector polyacrylamide gel electrophoresis Pesticide Analytical Manual, Volume I Pesticide Analytical Manual, Volume IL polychlorinated biphenyls principal components regression polymerase chain reaction photochemical differential calorimetry protein digestibility—cortected amino acid score portable document format polyether ether ketone protein efficiency ratio isoelectric point photoionization detector partial least squares Pasteurized Milk Ordinance photomultiplier tabe parts per billion Purchase Product Description parts per million parts per trillion pteroylglutamate polytetrafuomethyiene polyunsaturated fatty acids polyvinylpolypyrrolidone reference amount raw agricultural commodity rapid scan correlation Reference Daily Intake relative mobility radiofrequency reference dose red green blue refractive index radioimmunoassay Rapid One Step Assay Rebuttable Presumption Against Registration RapidViscoAnalyser revolutions per minute Saudi Arabian Standards Organization sD SDS SDS-PAGE SE SEC SEM. SEM. TMCS TINBS TOF SMS TSP TSUSA ie USDA US RDA uv UV-Vis Vis voc wt ww standard deviation sodium dodecy! sulfate sodium dodecy! sulfate-polyacrylamide gel electrophoresis standard error of the mean size-exchision chromatography scanning electron microscopy standard error of the mean solid fat content supercritical-fluid chromatography supercritical fluid extraction supercritical fluid extraction—gas chromatography solid fat index International Scientific selected ion monitoring safe level solid /liquid solids-not-fat solid-phase extraction solid-phase microextraction sulfite oxidase statistical quality control single residue methods swab test on premises thiobarbituric acid TBA reactive substances thermal conductivity detector tocopherol equivalents tetramethylethyienediamine thermogravimetric analysis total ion current thin-layer chromatography thermomechanical analysis trimethyichlorusilane trimethylsilyl trinitrobenzenesulphonic acid total organic carbon time-oFfight texture profile analysis total solids thermospray-mass spectrometry thermospray total soluble solids Tariff Schedules of the United States of ‘America United States Customs Service United States Department of Agriculture United States Recommended Dietary Allowance ultraviolet ultraviolet-visible visible volatile organic compounds weight wet weight basisGeneral InformationIntroduction to Food Analysis 14 Introduction 5 4.2 Trends and Demands 5 1.2.1 Consumers 5 1.2.2 Food industry 5 1.2.3 Government Regulations and International Standards and Policies 6 1.3 Types of Samples Analyzed 6 1.4 Steps in Analysis 6 1.4.1 Select and Prepare Sample 6 1.42 Perform the Assay 7 1.4.3 Calculate and Interpret tne Results| 7 1.8 Choice and Validity of Method 7 S. Suzanne Nielsen 1.8.1 Characteristics of the Method 7 1.5.2 Objective of the Method 7 1.8.3 Consideration af Food Composition and Characteristics 7 4.5.4 Validity of the Method 7 1.6 Oficial Methods 9 4.6.1 AOAC International 9 1.6.2 Other Endorsed Methods 10 1.7 Summary 11 4.8 Study Questions 12 1.9 References 12 4.10 Relevant Internet Addresses 12Chapter 1+ Introduction to Food Analysis 1.1 INTRODUCTION Investigations in food science and technology, whether by the ood industry, governmental agencies, or univer- sities, often require determination of food composition and characteristics. Trends and demands of consumers, the food industry, and national and international regu- Jations challenge food scientistsas they workto monitor food composition and to ensure the quality and safety of the food supply. All food products require analysis as part of a quality management program through- out the development process, through production, and after a product is in the market. The chemical com- position and physical properties of foods are used to determine the nutritive value, functional characteris- tics, and acceptability of the food product. The nature of the sample and the specific reason for the analy- sis commonly dictate the choice of analytical methods. Speed, precision, accuracy, and ruggedness often are key factors in this choice. Validation of the method for the specific food matrix being analyzed is neces- sary to ensure usefulness of the method. The success ‘of any analytical method relies on the proper selec- tion and preparation of the food sample, carefully performing the analysis, and doing the appropriate cal- culations and interpretation of the data. Methods of analysis developed and endorsed by several nonprofit scientific organizationsallow for standardized compar- isons of results between different laboratories, and for evaluation of less standard procedures. Such official methods are critical in the analysis of foods, to ensure that they meet the legal requirements established by governmental agencies. Government regulations and international standards most relevant to the analy- sis of foods are mentioned here but covered in mote detail in Chapter 2, and nutrition labeling regulations in the United States are covered in Chapter 3. Internet addresses for many of the organizations and govern- ment agencies discussed are given at the end of this chapter. 1.2 TRENDS AND DEMANDS. 1 Consumers have many choices regarding their food supply, so they can be very selective about the prod- ucts they purchase. They demand a wide variety of products that are of high quality, nutritious, and offer a good value. Also, consumers are concerned about the safety of foods, which has increased the testing of foods for allergens, pesticide residues, and prod- ucts from genetic modification of food materials. Many consumers are interested in the relationship between diet and health, so they utilize nutrient content and 4 Consumers. health claim information from food labels to make purchase choices. These factors create a challenge for the food industry and for its employees, For example, the demand for foods with lower fat content has chal- lenged food scientists to develop food products that contain fat content claims (e.g., free, low, reduced) and certain health claims (e.g, the link between dietary fat and cancer; dietary saturated fat and cholesterol and risk of coronary heart disease). Analytical methods to determine and characterize fat content provide thedata necessary to justify these statements and claims. Use of fat substitutes in product formulations makes possible many of the lower fat foods, but these fat substitutes, ‘can create challenges in the accurate measurement of fat content (1,2). 1.2.2 Food Industry To compete in the marketplace, food companies must produce foods that meet the demands of consumers as described previously. Management of product qual- ity by the food industry is of increasing importance, beginning with the raw ingredients and extending to the final product eaten by the consumer. Analytical ‘methods must be applied across the entire foad sup- ply chain to achieve the desired final product quality. Downsizing in response to increasing competition in the food industry often has pushed the responsibility for ingredient quality to the suppliers. Many companies have select suppliers, on whom they rely to perform the analytical tests to ensure compliance with detailed ingredient specifications. ‘Traditional quality control and quality assurance concepts are only a portion of a comprehensive quality management system. Food industry employees respon- sible for quality management work together in teams with other individuals in the company responsible for product development, production, marketing, and regulatory and consumer affairs. Analytical information must be obtained, assessed, and integrated with other relevant information about the food system to address quality-related problems, Making appropriate decisions depends on having knowledge of the analytical methods and equipment utilized to obtain the data related to the quality charac- teristics. To design experiments in product and process development, one must know the operating. princi- ples and capabilities of the analytical methods used. to assess results of the experiments to be conducted. Upon completion of these experiments, one must crit- ically evaluate the analytical data collected to deter- mine whether product reformulation is needed or what parts of the process need to be modified for future tests, The situation is similar in the research labo- ratory, where knowledge of analytical techniques is necessary to design experiments, and the evaluationPart * Generat Information of data obtained determines the next experiments to be conducted. 1.2.3 Government Regulations and International Standards and Policies ‘To market safe, high-quality foods effectively in a national and global marketplace, food companies must pay increasing attention to government regulations and guidelines, and to the policies and standards of international onganizations. Food scientists must be aware of these regulations, guidelines, and poli- cies related to food safety and quality, and know the implications for food analysis. Government regula- ‘ions and guidelines in the United States relevant to food analysis include nutrition labeling regulations (Chapter 3), Good Manufacturing Practice (GMP) regulations (Chapter 2), and Hazard Analysis Criti- cal Control Point (HACCP) systems (Chapter 2. The HACCP concept has been adopted not only by the United States Foad and Drug Administration (FDA) and other federal agencies in the United States, but also by the Codex Alimentarius Commission, an interna- tional organization that has become a major force in world food trade. Codex is described in Chapter 2, along with other organizations active in developing international standards and safety practices relevant to food analysis that affect the import and export of raw agricultural commodities and processed food products. 1.3 TYPES OF SAMPLES ANALYZED Chemical analysis of foods is an important part of a quality assurance program in food processing, from ingredients and raw materials, through processing, to the finished products 3-7). Chemical analysis also is important in formulating and developing new prod- ucts, and evaluating new processes for making food products, and in identifying the source of problems with unacceptable products (Table 1-1), For each type of product to be analyzed, it may be necessary to deter- mine either just one or many components. The nature of the sample and the way in which the information obtained will be used may dictate the specific method of analysis. For example, process control samples are usually analyzed by rapid methods, whereas nutri- tive value information for nutrition labeling generally requires the use of more time-consuming methods of analysis endorsed by scientific organizations. Critical ‘questions, including those fisted in Table 1-1, can be answered by analyzing various types of samples in a food processing system. Types of Samples Analyzed in a Quality Assurance Program for Food Products ‘Sample Type tical Questions Paw materials Do they mest your specticetons? ‘Dra sney sree Senne eg SRR CAITR, Wil a processing parameter have to be ‘modified because of any change in the composition of rew rnateials? ‘Ase the quaity and composition the same as for previous delvenies? How does the material from a potential naw ‘super compare to that from the current supplier? Process Did a speci procossing step resut in a control product of acceptable compostign or samples characterstics? Does a further processing step need to be modifed to obtain a fal product of acceptable aualiy? Finishea Doas it mest the lagal requirements? product What isthe nutritive value, so that label information can oe developed? Oris the naritive value as specitied on an esting label? Doss it meet product claim requirements fe.g., "low fat"? Wilt be acceptable to the consumer? ‘Will t have the appropriate sholf Ife? Competitor's What are ts composition and samols characteristics? How can we use this information to develop new procucts? Samp'aint How do the composition and characteristics sample ‘of a compan sarmple submitted by customer difie from a sample with 0 probiems? ‘Adapted and upsates tom @, 1.4 STEPS IN ANALYSIS: 1.4.1 Select and Prepare Sample Inanalyzing food samples of the types described previ- ously, all results depend on obtaining a representative sample and converting the sample 0 a form that can be analyzed. Neither of these is as easy as it sounds! Sampling and sample preparation are covered indetail in Chapter 5 Sampling is the initial point for sample identi- fication, Analytical laboratories must keep track of incoming samples and be able to store the analytical data from the analyses. This analytical information is stored on a laboratory information management system, or LIMS, which is a computer database program.Chapter 1» troduction to Food Analysis 1.4.2 Perform the Assay Performing the assay is unique for each component or characteristic to be analyzed and may be unique to a specific type of food product, Single chapters in this book address sampling and sample preparation (Chapter 5) and data handling (Chapter 4), while the remainder of the book addresses the siep of actually performing the assay. The descriptions of the vari ous specific procedures ate meant to be overviews of the methods, For guidance in actually performing the assays, details regarding chemicals, reagents, appa- ratus, and step-by-step instructions are found in the referenced books and articles. [¢ should be noted that numerous analytical methods utilize automated instra- mentation, including autosamplers and robotics, to speed the analyses, 1.4.3 Calculate and Interpret the Results To make decisions and take action based on the results, obtained from performing the assay that determined the composition or characteristics of a food product, one must make the appropriate calculations to inter- pret the data correctly. Data handling is covered in Chapter 4, 1.5 CHOICE AND VALIDITY OF METHOD 1.5.1 Characteristics of the Method Numerous methods often are available to assay food samples for a specific characteristic or component. To select or modify methods used to determine the chem- ical composition and characteristics of foods, one must be familiar with the principles underlying the pro- cedures and the critical steps. Certain properties of methods and criteria described in Table 1-2 are useful to evaluate the appropriateness of a method in current use or a new method being considered. 1.5.2 Objective of the Method Selection of a method depends largely on the objec- tive of the measurement. For example, methods used for rapid on-line processing meastirements may be less accurate than official methods (see section 1.6) used for nutritional labeling purposes. Methods referred to as reference, definitive, official, or primary are most appli- cable in a well-equipped and staffed analytical lab. The mote rapid secondary ot field methods may be more applicable on the manufacturing floor in a food pro- cessing facility. For example, refractive index may be used as a rapid, secondary method for sugar analy- sis (see Chapters 6 and 10), with results correlated to those of the primary method, high performance liq- itid chromatography (HPLC) (see Chapters 10 and 28) Moisture content data for a product being developed in the pilot plant may be obtained quickly with a mois- ture balance unit that has been calibrated using a more time-consuming hot air oven method (see Chapter 6), 1.5.3 Consideration of Food Composition and Characteristics Proximate analysis of foods refers to determining the major components of moisture (Chapter 6), ash (total minerals) (Chapter 7), lipids (Chapter 8), pro- tein (Chapter 9), and carbohydrates (Chapter 10). The performance of many analytical methods is affected by the food matrix (Le, its major chemical components, especially lipid, protein, and carbohydrate). For exam ple, high-fat or high-sugar foods can cause different types of interferences than low-fat or low-sugar foods. Digestion procedures and extraction steps necessary for accurate analytical results can be very dependent on the food matrix. The complexity of various food systems often requires having not just one technique available fora specific food component, but multiple techniques and procedures, as well as the knowledge about which to apply to a specific food matrix. ‘A task force of AOAC International, formerly known as the Association of Official Analytical Chemists (AAC), suggested a “triangle scheme" for dividing foods into matrix categories (10-12) (Fig, 1-1). ‘Theapexesof the triangle contain food groups that were either 100% fat, 100% protein, or 100% carbohydeate. Foods were rated as “high,” “low,” or “medium” based on levels of fat, carbohydrate, and proteins, which are the three nutrients expected to have the strongest effect, on analytical method performance. This created nine possible combinations of high, medium, and low lev ls of fat, carbohydrate, and protein. Complex foods ‘were positioned spatially in the triangle according to their content of fat, carbohydrate, and protein, on a normalized basis (ie., fat, carbohydrate, and protein normalized to total 100%), General analytical methods ideally would be geared to handle cach of the ninecom= binations, replacing more numerous matrin-dependent methods developed for specitic foods. For example, using matrix-dependent methods, one method might be applied to potato chips and chocolates, which are both low-protein, medium-fat, medium-carbohydrate foods, but another might be required for a high-protein, low-fat, high-carbohydrate food such as nonfat dry ‘milk (2D. In contrast, a robust general method could ‘be used for all of the food types. The American Asso- ciation of Cereal Chemists (AAC) has approved a ‘method studied using this approach (12). 1.5.4 Validity of the Method Numerous factors affect the usefulness and valid- ity of the data obtained using a specific analytical method. One must consider certain characteristics of8 Part © General information tab! Crtlaria for Choice of Food Analysis Methods Sharasterieve ‘Crlical Questions inherent properties: # Speciicity’Secctivty Is the property being measured the sarne as that claimed to be measured, ands it te only progerty being measured? ‘Ara there interferences? ‘What stops aro boing taken to ensure a high degres of specifiy? « Precision What is the precision of the method? Is there withn-batch, batch-to-bateh, or day-to-day variation? ‘What step in the procedure contributes the greatest variably? Accuracy How does the new method compare in accuracy to the old or @ standard method? What is the percent recovery? Anpiicabilty of method tc laboratory # Sample size How much samie is needed? Isit too large or too small to ft your needs? Doss it ft your equipment and/or glassware? = Reagents Gan you propery prepare ther? \Wral equipment is needed? Are they stabi? For how long and under what ‘conditions? # Ecuipment Is the method very sensitive to slight or moderate changas in the reagents? Do you have the appropriate equpment? ‘Are personnal compatent to operate equipment? = Cost ‘What is the cost in terms of oguioment, reagents, and personnel? Usefuiness Time required How fastie i? How fast does it nec to bs? Reiabilty Hew reliable ist from the standpoints of precision and stability? = Nese: Does it meet a need or vetter mest anaed? Is any change in method wort the rouble of the change? Personne © Safety ‘Are spacial precautions necessary? © Procedures ‘Who will repre the written description of the procedures and reagents? Who will do any required calculatons? Fat 100% fat ho at 39% 400% Ty a % cordate Frnt RE Att cartes PARSE ARRAN, PEE Schematic layout of food matrixes based on protein, fat, and carbohydrate content, exchuding moisture and ash paren] Reprinted with permission froty (13, Insite Lahortony Management, September 1997, p. 33, Copyright 1987, by AOAC International‘Chapter 1 ® Introduction to Food Analysis. any method, such as specificity, precision, accuracy, and sensitivity (see Table 1-2 and Chapter 4). How- ever, one also imust consider how the variability of data from the method for a specific characteristic compares to differences detectable and acceptable to a consumer, and the variability of the specific characteristic inher- ent in processing of the food. One must consider the nature of the samples collected for the analysis, how representative the samples were of the whole, and the number of samples analyzed (Chapter). One must ask whether details of the analytical procedure were fol- lowed adequately, such that the results are accurate, repeatable, and comparable to data collected previ- ously For data to be valid, equipment to conduct the analysis must be standardized and appropriately used, and the performance limitations of the equipment recognized. A major consideration for determining method validity is the analysis of materials used as controls, often referred to as standard reference materials or check samples. Standard reference materials can be obtained in the United States from the National Insti- tute of Standards and Technology (NIST), in Canada from the Center for Land and Biological Resource Research, in Europe from the Institute for Reference Materials and Measurements (IRMM), and in Belgium from the Community Bureau of Reference (BCR). Numerous organizations offer check sample services that provide test samples to evaluate the reliability of a method (14). For example, the AACC has a check sam- ple service in which a subscribing laboratory receives specifically prepared test samples from AACC. The subscribing laboratory performs the specified analy- ses on the samples and returns the results to AACC. The AACC then provides a statistical evaluation of the analytical results and compares the subscribing labora- tory’s data with those of other laboratories to inform the subscribing laboratory of its degree of accuracy. The AACC offers check samples such as flours and semolina, for the analysis of vitamins and minerals, sugars, sodium, total dietary fiber, soluble and insol- uble dietary fiber, f-glucan, near-infrared analyses, sanitation, and microbiology. ‘The American Oil Chemists’ Society (AOCS) has a check sample program for oilseeds, oilseed meals, marine oils, aflatoxin, trans fatty acids, oils/fats, and various oil and fat constituents. Laboratories from many countries participate in the program to check the accuracy of their work, their reagents, and their lab- oratory apparatus against the statistical norm derived from the group data. Standard reference materials are important tools to ensute reliable data, However, such materials need not necessarily be obtained from outside organiza- Hions, Control samples internal to the laboratory can be prepared by carefully selecting an appropriate type of sample, gathering a large quantity of the material, mixing and preparing to ensure homogeneity, packag- ing the sample in small quantities, storing the samples appropriately, and routinely analyzing the control sample when test samples are analyzed. Whatever the standard reference materials used, these should match closely the matrix of the samples to be analyzed by a specificmethod. AOAC International has begun a peer- review program of matching reference materials with respective official methods of analysis, 1.6 OFFICIAL METHODS The choice of method for a specific characteristic or component of a food sample is often made easier by the availability of official methods. Several nonprofit, scientific organizations have compiled and published these methods of analysis for food products, which have been carefully developed and standardized. They allow for comparability of results between different laboratories that follow the same procedure, and for evaluating results obtained using new or more rapid procedures, 1.6.1 AOAC International AOAC International is an organization begun in 1884 to serve the analytical methods needs of government regulatory and research agencies. The goal of AOAC International is to provide methods that will be fit for their intended purpose (ic,, will perform with the nec- essary accuracy and precision under usual laboratory conditions). This volunteer organization functions as follows: 1, Methods of analysis from published literature are selected or new methods are developed by AOAC International volunteers. 2. Methods are collaboratively tested using multi- laboratory studies in volunteers’ laboratories. 3. Methods are given a multilevel peer review by expert scientists, and if found acceptable, are adopted as official methods of analysis. 4. Adopted methods are published in the Official ‘Methods of Analysis, which covers a wide variety of assays related to foods, drugs, cosmetics, agri- culture, forensic science, and products affecting public health and welfare. 5. AOAC International publishes manuals, meth- ‘ods compilations in specific areas of analysis, monographs, and the monthly magazine Inside Laboratory Management. 6. AOAC International conducts training courses of interest to analytical scientists anct other lab- oratory personnel.10 ‘Methods validated and adopted by AOAC Interna- tional and the data supporting the method validation are published in the Journal of AOAC International. Such methods must be successfully validated in @ for- mal interlaboratory collaborative study before being accepted as an official first action method by AOAC International. Details of the validation program (eg., number of laboratories involved, samples per level of analyte, controls, control samples, and the review process) are given in the front matter of the AOAC International's Official Methods of Analysis. First action methods are subject to scrutiny and general testing by other scientists and analysts for some time period before final action adoption. Adopted first action and final action methods are compiled in books published and updated every four to five years as the Official ‘Methods of Analysis (15) of AOAC International. Supple- menisto the book are published yearly and contain new methods and revisions to current methods. The Off- cial Methods of Analysis of AOAC International includes methods appropriate fora wide variety of products and other materials (Table 1-3), These methods often are specified by the FDA with regard to legal requirements for food products. They are generally the methods followed by the FDA and the Food Safety and Inspec- tion Service (FSIS) of the United States Department of Agriculture (USDA) to check the nutritional label- ing information on foods and to check foods for the presence or absence of undesirable residues or residue levels. 1.6.2 Other Endorsed Methods The AACC publishes a set of approved labora- tory methods, applicable mostly to cereal products (eg, baking quality, gluten, physical dough tests, staleness /texture). The AACC process of adopting the Approved Methods of Analysis (16) is consistent with the ‘process used by the AOAC International and AOCS. ‘Approved methods of the AACC are continuously reviewed, critiqued, and updated (Table 1-4). They are printed in a looseleaf format, contained in ring binders. Supplements containing new and revised procedures are provided annually. ‘The AOCS publishes a set of official methods and recommended practices, applicable mostly to fat and oil analysis (e.g., vegetable oils, glycerin, lecithin) (17) (able 1-5). AOCS is a widely used methodology source on the subjects of edible fats and oils, oilseeds and oilseed proteins, soaps and synthetic detergents, indus- trial fats and ofls, fatty acids, oleochemicals, glycerin, and lecithin. Standard Methods for the Examination of Dairy Pro ucts (18), published by the American Public Health Association, includes methods for the chemical analy- sis of milk and dairy products (e.g., acidity, fat, lactose, Part| ¢ General Information Teibie of Contonts of 2000 Orficla! Methods [tente_| of Analysis of AOAC Intemational (15) Chapter Tite 1 Agricuture liming materials 2 Fertiizers 8 Prants 4 Animal feed 5 Drugs in feeds @ Disivectants 7 Posticide forrrulations 8 Hazardous substances 9 Metals and other elements at trace levels in foods 10 Pasticide anc industrial chemical residues ii Waters; anc salt 12 Micrechemical methods 18 Radioactuty 14 Veterinary analytical toxicology 18 Cosmetics 16 Extrenecus materials: Isolation 7 Microbiological methods: 18 Drugs: Pet! 19 Drugs: Pert I 20 rugs: Part il 21 Drugs: Part IV 22 Drugs: Part V 2 Drugs and feed! adoitives in animal issues 2a Forensic sciences 28 Baking powders and baking chernioals 26 Distiled tiquors. 27 Mait beverages and brewing materia's 28 Wines: 2 ‘Nonalcoholic beverages and concentrates 30 Coffee and lea a Cacao bean and its products 82 Coreal foods 38 Dary products 34 Eggs and egg products 38 Fish and other marine products 36 Flavors 37 Fruits and uit products 38 Gelatin, dessert preparations, anc mixes 39 Meat and meat products 40 Nuts and nat products 4 Gils and fats 42 Vegetable products, processed 3 Spices and other condiments 44 ‘Sugars and sugar products, 45 Vitamins and other nutrients 48 Color additives a7 Food additives: Direct 48 Food addives: Indirect 49 Netural toxins 50 Infant forrrulas, baby foods, and enteral products moisture/solids, added water) (Table 1-6). Standard ‘Methods for the Examination of Water and Wastewater (19) is published jointly by the American Public Health Association, American Water Works Association, and the Water Environment Federation. Food Chemicals Codex (20), published by the Food and Nutrition Board of the National Research Council/National AcademyChapter 1 ® Introduction to Food Analysis " Table of Contents of 2000 Approved FEZ Methods of the American Association of Table of Contents of 1998 Otticial Methods ‘and Recommended Practices of the [tate | Cereal Chemists (15) American Olt Chemists’ Society (16) Chapter Tite Section Tite 2 Acidity A Vegstabie ol source materials 4 ods B ——Olbeed by-products 6 ‘Admninture of fours © Gommerical fats and cls 7 ‘Amino acids D Soap and syrthetis detergents e Total ash — Glycerin 10 Baking quality F Sulfonated and sulfated cits 1 Blotechnology G ——_Scapsiocks 12 Cartoon dioxide H Specifications tor reagents, solvents, anc apparatus 14 Calor and pigments J Lectria 20 Ingredients, M ———_Evakalon and dasign of test methods 22 Engyines S Official stings 26 Experimental millng T iscomended practices for tasting industrial os 28 [Exireneous matter and derivatives 80, Crude fat a2 Foe 33 Sensory analysis, 38 Guuton 39 Infrared analysis Contents of Chapter 15 on 40 Inorganic constituents ‘Chemical and Physical a Microorganisms Methods In Standard Methods a4 Moisture for the Examination ot Dairy 45 Myootoxins Products (18) 48 Nitrogen 48 Oxidizing, bleaching, and maturing agents Intredation 4 Physical Gough tests Acidity tests 55 Physica tests ‘Adultorant tests 58 Prysicochemical tests Ash tests 8 ‘Special properties of fats, ois, and shortonings Chior ce (salt tests 6 Price ‘Contaminant teste 62 Preperation of sample Bdiraneous materi tests ea sampling Fat tosts 6 Semoina, pasta, anc noodle quaity Lactose/galactoss tests 8 Solutions Minerals and food adctves 1% Stalenessitextura Mostura/soleis test's 8 Starch Multicomponent tosts 8 Statstical principles Protenintrogen tests 0 Sugars Rancidiy tests 2 Tables Sanitizer tests 86 Vearvins Vitarnin tests 69 Yoast of Science, contains methods for the analysis of cer- tain food additives, Some trade associations publish standard methods for the analysis of their specific products. 1.7 SUMMARY Food scientists and technologists determine the chem- ical composition and physical characteristics of foods routinely as part of their quality management, product development, or research activities. For example, the types of samples analyzed in a quality management Program ofa food company can include raw materials, Functional tests process control samples, finished products, competi- tors’ samples, and consumer complaint samples. Con- sumer, food industry, and government concern for food quality and safety has increased the importance of anal- yses that determine composition and critical product characteristics To successfully base decisions on results of any analysis, one must correctly conduct all three major steps in the analysis; (1) select and prepare samples, (2) perform the assay, and (3) calculate and interpret the results. The choice of analysis method is usually ‘based on the objective of the analysis, characteristics of the method itself (e.g, specificity, accuracy, precision, speed, cost of equipment, and training of personnel),12 Part! © General Information and the food matrix involved. Validation of the method is important, as is the use of standard reference mate- rials to ensure quality results. Rapid methods used for quality assessment in a production facility may be less accurate but much faster than official methods used for ‘nutritional labeling. Endorsed methods for the chemi- calanalyses of foods have been compiled and published by AOAC International, AACC, AOCS, and certain other nonprofit scientific orgonizations. These meth- ‘ods allow for comparison of results between different laboratories and for evaluation of new or more rapid procedures. 1.8 STUDY QUESTIONS 1. Identify six reasons you might need to determine certain chemical characteristics of a food product as part of a quality management program. 2. You are considering the use of a new method to measure Composind Xin your food product. List sx factors you will consider before adopting this new method in your quality assurance laboratory. 3. In your work at a food company, you mentioned to a co worker something about the Official Methads of Analysis published by AOAC International, The co-worker asks ‘yout what the term “AOAC” refers to, what AOAC Inter- rational doxs, and what the Official Metts of Analysis is, Answer your co-worker's questions. 4. For each type of product listed below, identify a publica tion in which you can find standard methods of analysis appropriate for the product b. enriched flour <¢ wastewater (rom fond pressing plant) 4. margarine. 1.9 REFERENCES 1. Kirchner, E.M. 1997, Fake fats in real fond. Chemical & Engineering Neves 75(16): 19-25, 2. Flickinger, B. 1997. Challenges and solutions in composi- tional analysis. Food Quaity 329): 21-26. 3. Stauffer, JF, 1988. Quality Assurance of Fant Ingredi- ents, Processing and Distribution, Food 6 Nutrition Press, Westport, CT. 4, Gould, WA. 198. Total Quality Assurance for the Foot Indusivies, Teehvomic, Lancaster, PS. 5 Malton, JL. 1995, Analysis and Contr? Methods for Foods and Agricultural Products. Vol. 1. Quality Conirol for Foods aud Agricultural Products, John Wiley & Sons, New York. 6. Linden, G, and Hurst, WJ. 1996. Anaiysis and Control ‘Methods for Foods ond Agricultaral Products. Vol. 2. Ante {ytical Teckniques for Foods act Agricultural Products, Toh Wiley & Sons, New York 7. Multon, J-L, Stadleman, WJ. and Watkins, B.A. 1997 Analysis and Control Methods for Foods and Agricultural Products. Vol. 4. Analysisof Fond Constituens, John Wiley & Sons, New York, 8, Pearson, D. 1973. Introduction—Some basic principles Cf quality control. Ch. 1, in Laboratory Techniques tn Food Analysis, 1-26, John Wiley & Sons, New York. 9. Pomeranz, Y, and Meloan, CE, 1994, Food Analysis Theory and Prectice, 3rd ed. Chapman & Hall, New York. 10. AOAC International, July 1993. A food matrix organiza tional system applied to collaborative stadies. The Referee 1701, 6,7. 11, Lovett, RA. 1997. US. food label law pushes fringes of analytical chemistry. Inside Laborniory Management Va) 27-28. 12, DeVries, W., and Silvera, KR. 2001, ACC collaborative: study of a method for determining vitamins A and E in foods by HPLC (AACC Method 86-06). Cert Fos Wild 4665): 211-215, 13, Bilis, C, Hite, D., and van Egmond, H. 1997. Develop: ‘ment of methods to test all food matrixes unrealistic, ays OMB. Irs Laboratory Management 18): 33-35. M4. Latimer, GW, Jr. 1997, Check sample programs keep laboratories in syne. hiside Lateratory Management 1% 18-20. 15. AOAC International. 20"), Official Methods of Analysis, ‘Vth ed. AOAC Intemational, Gaithersburg, MD. 16. ACC. 2000. Approved Methods of Artalusis, 1th ed. “American Association of Cereal Chemists, St, Panl, MN. 17, AOCS. 1998. Official Methods of Recommended Practices, 5th ed. (1999 and 2089/2001 Additions and Revisions) American Oil Chemists’ Society, Champaign, IL 18, Wehr, HLM, and Frank, JF (Eds), 2002, Standard Metis Jor the Examination of Dairy Products, 17th ed. American Public Health Association, Washington, DC. 19, Clesceri, LS, Greenberg, AE, and Paton, A.D, (Eds). 1998, ‘Standard Methods for the Examination of Water and Wastewater, 20th ed, American Public LIcalth ‘Association, Washington, DC. 20, National Academy of Sciences, 199%, Foot Chem jocls Cadex, 4th ed, Food and Nutrition Board, National Research Council, National Academy Press, Washington, DC. 1.19 RELEVANT INTERNET ADDRESSES American Association of Cereal Chemists hitp:/ /wwwscisoc.org/aacc/ American Oil Chemists’ Society http://www.aoes.org/ American Public Health Association hitp:/ /wwwaphaorg/ AOAC Intemational hitp:/ /www.aoac.org, Code of Federal Regulations http: /wwwaccess.gpo gov /nata/cit/ cfr-table-search html Codex Alimentarius Commission hitp:/ /www.codexalimentarius.net/Chapter 1 = ntroduetion to Food Analysis 13 Food Chemicals Codex http: / /www?2.nas.edu/codex Food and Drug Administration http://wwwda.gov Center for Food Safety & Applied Nutrition http: / /vi.cfsan.fda.gov /list.html Current Good Manufacturing Practices itp: /efsan fda gov/~dms/dscgmps.html Food Labeling and Nutrition http: //vm.cfsan fda gov/label html Hazard Analysis Critical Control Point hitp:/ /vm.cfsan.fda.gov/~Ird/hacepsub.htmnl National Institute of Standards and ‘Technology hitp:/ /wwwanist.gov/ US. Department of Agriculture http:/ /www.usda.gov Food Safety and Inspection Service hittp:/ /www.fsis.usda.gov HACCP/Pathogen Reduction http:/ /www.gov/oa/haccp/yi United States Government Regulations and International Standards Related to 2.4 Introduction 17 2.2 United States Federal Regulations Atfecting Food Composition 17 2.2.1 United States Food and Drug Administration (FDA) 17 2.2.4.4 Legislative History 17 2.2.1.1.1 Federal Food, Drug, and Cosmetic Actof 1938 17 2.2.1.1.2 Amendments and Additions to the 1938 FD&C Act 17 Food Analysis S. Suzanne Nielsen 2.2.1.4.8 Other FDA Regulations 18 2.2.1.2 Food Definitions and Standards 18 2.2.1.3 Inspection and Enforcement 18 2.2.2 Unted States Department of Agriculture 21 2.2.2.1 Standards of Identity for Meat Products 21 2.2.22 Grade Standards 21 2.2.2.3 Inspection Programs 21 2.2.8 United States Department of Commerce 22 22.3.1 Seafood Inspection Service 2216 Part © General information 2.2.9.2 Interaction with FDA and EPA 22 2.2.4 United States Bureau of Alcohol, Tobacco, Firearms, and Explosives 22 2.2.4.1 Regulatory Responsibility for Alcoholic Beverages 22 2.2.4.2 Standards and Composition of Beer, Wine, and Distiled Baverage Spirits 22 2.2.5 United States Environmental Protection Agency 23 22.5.1 Pesticide Registration and Tolerance Levels 23 22.52 Drinking Water Standards and Contaminants 23 2.2.58 Effluent Composition trom Food Processing Plants 24 2.2.6 United States Customs Service 24 2.2.6.1 Harmonized Tari Schedule of the United States (TSUSA) 25 2.2.6.2 Food Composition and the TSUSA 25 2.2.7 United States Federal Trade Commission 25 2.2.7.1 Enforcement Authority 25 2.2.7.2 Food Labels, Food Composition, and Deceptive Advertising 25 2.3 Regulations and Recommendations for Milk 26 2.8.1 FDARosponsibiliies 26 2.9.2 USDA Responsibilities 26 2.3.8 State Responsibilities 27 2.4 Regulations and Racomnendations for Shelfish 27 2.4.1 Stato and Federal Sheltish Sanitation Programs 27 2.4.2 Natural an Environmental Toxic Substances in Shellfish 27 2.5 Voluntary Federal Recommendations Aflecting Food Composition 28 2.8.1 Food Specifications, Food Purchase, and Government Agencies 28 2.5.2 National Conference on Weights and Measures State Food Packaging Regulations 28 2.6 International Standards and Policies 28 2.6.1 Codex Alimentarius 29 2.6.2 ISO Standards 29 2.6.3 Other Standards 30 27 Summary 30 2.8 Study Questions 30 2.9 References 31 2.10 Relevant Internet Addresses 32Chaplet 2 United States Government Reguiations 7 2.1 INTRODUCTION Knowledge of government regulations relevant to the chemical analysis of foods is extremely important to persons working in the food industry. Federal laws and regulations reinforce the efforts of the food indus- try to provide wholesome foods, to inform consumers about the nutritional composition of foods, and to elim- inate economic frauds. In some cases, they dictate what ingredients a food must contain, what must be tested, and the procedures used to analyze foods for safety fac- tors and quality attributes. This chapter describes the United States federal regulations related to the compo- sition of foods, The reader is referred to references 1-4 for comprehensive coverage of United States food laws and regulations. Many of the regulations referred to in this chapter are published in the various Titles of the Code of Federal Regulations (CER) (5). This chapter also includes information about food standards and safety practices established by international organizations Internet addresses are given at the end of this chapter for many of the government agencies, organizations, and documents discussed 2.2 UNITED STATES FEDERAL REGULATIONS AFFECTING FOOD COMPOSITION 2.2.1 United States Food and Drug Admintatration (FDA) ‘The FDA is a US. government agency within the Department of Health and Human Services (DHHS) ‘The FDA is responsible for regulating, among other things, the safety of foods, cosmetics, dnigs, medical devices, biologicals, and radiological products. It acts under laws passed by the United States Congress to monitor the affected industries and ensure the con- sumer of the safety of such products. A comprehensive collection of federal laws, guidelines, and regulations relevant to foods and drugs has been pubtished by the Food and Drug Law Institute (2). 22.1.1 Legislative History 2.2.1.1.1 Federal Food, Drug, and Cosmetic Act of 1938 TheFederal Food, Drug, and Cosmetic FD&C) Act of 1938 was intended to assure consumers that foods are safe and wholesome, produced under sani- tary conditions, and packaged and labeled truthfully. This law, which broadened the scope of the Food and Drug Act of 1906, further defined and set regulations on adulterated and misbeanded foods. The FDA was given power to seize illegal products and to imprison and fine violators. An important part of the 1938 Act relevant to food analysis is the section that authorizes food definitions and standards of identity, as further described below, 22.1.1.2 Amendments and Additions to the 1938 FD&C Act The 1938 FD&C Act has been amended several times to increase its power. The Miller Pes- ticide Amendment was added in 1954 to specify the acceptable amount of pesticide residues on fresh fruits, vegetables, and other raw agricultural products when they enter the marketplace. This Amendment, then under the authority of the FDA, is now administered by the Environmental Protection Agency (EPA). ‘The Food Additives Amendment enacted in 1958 was designed to protect the health of consumers by requiring a food additive to be proven safe before addi- tion to a food and to permit the food industry to use food additives that are safe at the intended level of use. The highly controversial Delaney Clause, attached as a rider to this amendment, prohibits the FDA from set- lingany tolerance level asa food additive for substances, known to be carcinogenic. The Color Additives Amendment of 1960) defines color additives, sets rules for both certified and uncerti- fied colors, provides for the approval of color additives, that must be certified or are exempt from certifica- tion, and empowers the FDA to list color additives for specific uses and set quantity limitations. Similar to the Food Additives Amendment, the Color Additives Amendment contains a Delaney Clause. ‘The Nutrition Labeling and Education Act of 1990 (NLBA), described further in Chapter3, made nutrition labeling mandatory on most food products under FDA jurisdiction, and established definitions for health and, nutrient claims, The NLEA emphasized the relation- ship between diet and health, and provided consumers a means to choose foods based on complete and truthful label information. ‘The Dietary Supplement Health and Education Act (1994) (DSHEA) changed the definition and reg ulations for dietary supplements from those in the FD&C Act and in acts relevant to dietary supplements passed prior to 1994. The DSHEA defined supplements as “dietary ingredients” (defined in specific but broad, terms), set criteria to regulate claims and labeling, and established government agencies to handle regulation. Classified now as "dietary ingredients” rather than by the previously used term “food additives,” dietary sup- plements are not subject to the Delaney Clause of the FD&C Act. Regulations for dietary supplements permit claims not allowed for traditional foods. Control and regulation of dietary supplements have been separated from those for traditional foods. ‘The Food Quality Protection Act (1996) amended both the FD&C Act and the Federal Insecticide,18 Part * Genera Information Fungicide and Redenticide Act (FIFRA), as further described in section 2.25.1. 2.2.1.1.3 Other FDA Regulations ‘TheFDA hasdevel- ‘oped many administrative rules, guidelines, and action levels, in addition to the regulations described above, to implement the FD&C Act of 1938. Most of them are published in Title 21 of the CFR. They include the Good Manufacturing Practice (GMP) regulations (21 CFR 110), regulations regarding food labeling (21 CFR 101), recall guidelines (21 CFR 7.40), and nutritional quality guidelines (21 CFR 104). The food labeling reg ulations include nutritional labeling requirements and guidelines, and specific requirements for nutrient con~ tent, health claims, and descriptive claims (discussed in Chapter 3). ‘With increasing responsibility being placed on food processors and regulatory agencies to ensure the safety of foods eaten by consumers, FDA has placed consid- erable emphasis on GMP regulations and on Hazard Analysis Critical Control Point (HACCP) systems. HACCP is an important component of an interagency initiative to reduce the incidence of foodborne illness, and includes the FDA, USDA, EPA, and the Centers for Disease Control (CDC) (6). Both GMP and HACCP sys- tems emphasize the importance of preventing hazards, toavoid problems associated with detecting hazards in foods. ‘The GMP regulations, legally based on the FD&C Act, but not established as a proposed rule until 1969, ate designed to prevent adulterated food in the market- place (7, 8). The GMP regulations define requirements for acceptable sanitary operation in food plants and include the following relevant to food processing: 1. General provisions that define and interpret the detailed regulations; 2, Requirements and expectations for maintaining grounds, buildings and facilities; 3, Requirements and expectations for design, con- struction, and maintenance of equipment; 4, Requirements for production and process con- trols; and 5. Defect action levels (DALs) for natural and unavoidable defects. In addition to general GMPs (21 CFR 110), specific GMPs exist for thermally processed low-acid canned foods @1 CFR 113), acidified foods (21 CFR 114), and bottled drinking water (21 CFR 129). Unlike GMP regulations, HACCP is a system developed and implemented by a food processor, orig- inally designed to produce zero defect (no hazard) food for astronauts to consume on space flights (9). The FDA, and USDA have adopted the HACCP concept in cer- tain of their inspection programs. An effective HACCP, program has the following components: 1, Determine potential hazards in each process, 2. Identify critical control points, 3. Establish control limits for each critical control point. 4. Establish procedures to monitor control points. 5, Establish corrective actions when limits of con- trol point are exceeded, 6. Establish appropriate system of record keeping. 7. Establish program to verify efficacy of program. While GMPs and HACCP programs are based largely ‘on microbiological concerns, certain chemical and physical tests (eg., inactivation of toxic constituents, presence of extraneous matter, metal detection) are ‘often necessary to ensure the safety of foods. 2.2.1.2 Food Definitions and Standards The food definitions and standards established by the FDA are published in 21 CFR 100-169 and includestan- dards of identity, quality, and fill. The standards of identity, which have been set for a wide variety of food products, are most relevant to the chemical anal- ysis of foods because they specifically establish which ingredients a food must contain, They limit the amount of water permitted in certain products. The minimum levels for expensive ingredients are often set, and max- imum levels for inexpensive ingredients are sometimes set. The kind and amount of certain vitamins and min- crals that must be present in foods labeled “enriched” are specified. The standards of identity for some foods include a list of optional ingredients. The standard of identity for sour cream (21 CFR 131,160) is given in Fig, 2-1. Table 2-1 summarizes the standards of iden- tity relevant to food analysis for a number of other foods. Note that the standard of identity often includes, the recommended analytical method for determining chemical composition, Although standards of quality and fill are less related to the chemical analysis of foods than are stan- dards of identity, they are important for economic and quality control considerations. Standards of quality, established by the FDA for some canned fruits and veg- tables, set minimum standards and specifications for factors such as color, tenderness, weight of units in the container, and freedom from defects. The standards of {ill established for some canned fruits and vegetables, tomato products, and seafood state how fulla container must be to avoid consumer deception. 2.2.1.3 Inspection and Enforcement ‘The FDA has broadest regulatory authority over most foods (generally, all foods other than meat, poultry, ‘eggs: water supplies; imported foods). However, the