U.S. Food & Drug Administration
Center for Food Safety & Applied Nutrition

FDA Technical Bulletin Number 5
Macroanalytical Procedures Manual
1984; Electronic Version 1998


The Macroanalytical Procedures Manual is currently being revised to update its content and add new material. In the interim, we have converted the original 1984 edition of the manual for display on the FDA website. This website version was produced as a cooperative effort between the editors and the Center for Food Safety and Applied Nutrition (CFSAN). Our purpose is to provide access to the out-of-print 1984 manual until the revised edition is available.

TABLE OF CONTENTS


Editor's Preface
I. INTRODUCTION I-1
  (1) Definition of Macroanalytical Methods I-1
  (2) Advantages and Limitations of Macroanalytical Methods I-1
  (3) Scope of the Macroanalytical Procedures Manual I-2
  (4) Legal Aspects I-2
  (5) Determination of Defects I-1
  (6) Sampling Methods I-1
II. APPARATUS FOR MACROANALYTICAL METHODS II-1
III. REAGENTS FOR MACROANALYTICAL METHODS III-1
IV. SPECIAL TECHNIQUES IV-1
  (1) X-Ray Radiography IV-1
  (2) Determination of the Direction of Insect Penetration of Food Packaging IV-2
  (3) Microscopic Confirmation of Decomposition and Rot IV-4
  (4) Detection and Recovery of Live Insects IV-4
V. MACROANALYTICAL METHODS V-1
  1. BEVERAGE AND BEVERAGE MATERIALS V-1
    A. METHOD FOR COFFEE BEANS V-1
  2. BAKERY PRODUCTS, CEREALS, AND ALIMENTARY PASTES V-12
    A. A. METHOD FOR BAKERY PRODUCTS, COOKED CEREALS, AND ALIMENTARY PASTES V-12
    B. METHOD FOR MODIFIED WHOLE GRAINS V-13
  3. GRAINS AND GRAIN PRODUCTS V-15
    A. METHOD FOR WHEAT, CORN, AND OTHER GRAINS V-15
  4. CHOCOLATE, SUGARS, AND RELATED PRODUCTS V-18
    A. METHOD FOR COCOA BEANS V-18
    B. METHOD FOR CANDY V-22
  5. MISCELLANEOUS AND MULTIPLE FOOD PRODUCTS V-24
    A. METHOD FOR PLANT GUMS V-24
  6. DAIRY, CHEESE, AND RELATED PRODUCTS V-26
    A. METHOD FOR CASEIN AND SODIUM CASEINATE V-26
  7. SEAFOOD V-27
    A. METHOD FOR MICROSCOPIC DETECTION OF FISH TISSUE IN CRAB MEAT OR CRAB CAKES V-27
    B. METHOD FOR DETERMINATION OF PARASITESIN FIN FISH V-28
  8. SPICES, CONDIMENTS, FLAVORS, AND CRUDE DRUGS V-32
    A. GENERAL METHOD FOR SPICES, HERBS, AND BOTANICALS V-32
    B. SUPPLEMENTAL METHOD FOR BLACK AND WHITE PEPPER V-39
    C. SUPPLEMENTAL METHOD FOR NUTMEGS V-41
  9. FRUITS AND FRUIT PRODUCTS V-42
    A. METHOD FOR APPLE PRODUCTS V-42
    B. METHOD FOR DECOMPOSITION IN BLACKBERRIES, RASPBERRIES AND OTHER DRUPELET BERRIES V-44
    C. METHOD FOR DECOMPOSITION IN BLUEBERRIES V-46
    D. METHOD FOR CHERRIES V-48
    E. METHOD FOR CANNED AND FROZEN FRUITS V-51
    F. METHOD FOR DRIED FRUITS V-53
    G. METHOD FOR GRAPE PRODUCTS V-59
    H. METHOD FOR JAMS, PRESERVES, AND JELLIES V-61
    I. METHOD FOR LINGONBERRIES V-64
    J. METHOD FOR MINCEMEAT V-66
    K. METHOD FOR OLIVES V-67
    L. METHOD FOR PINEAPPLE PRODUCTS V-73
    M. METHOD FOR RAISINS V-76
    N. METHOD FOR PROCESSED STRAWBERRIES V-78
  10. NUTS AND NUT PRODUCTS V-81
    A. METHOD FOR IN-SHELL AND SHELLED TREE NUTS V-81
    B. METHOD FOR PEANUTS AND PEANUT SIFTINGS V-89
    C. METHOD FOR MICROSCOPIC DETECTION OF FOREIGN PLANT TISSUES IN PEANUT BUTTER V-92
  11. VEGETABLES AND VEGETABLE PRODUCTS V-93
    A. METHOD FOR ASPARAGUS V-93
    B. METHOD FOR BRUSSELS SPROUTS V-95
    C. METHOD FOR MICROSCOPIC DETECTION OF SUBSTITUTE VEGETABLE TISSUES IN GROUND HORSERADISH V-96
    D. METHOD FOR LETTUS V-98
    E. METHOD FOR MUSHROOM PRODUCTS V-100
    F. METHOD FOR THE PRESERVATION AND IDENTIFICATION OF MUSHROOMS V-102
    G. METHOD FOR PEAS AND BEANS (CANNED, FROZEN, AND DRIED) V-104
    H. METHOD FOR PICKLED VEGETABLES AND RELISH V-108
    I. METHOD FOR PIMIENTOS V-111
    J. METHOD FOR POTATO CHIPS V-113
    K. METHOD FOR CORN HUSKS V-115
    L. METHOD FOR GARLIC BULBS V-117
  12. COSMETIC PRODUCTS V-119
    A. METHOD FOR COSMETIC BRUSHES V-119
VI. APPLICATIONS OF MACROANALYTICAL METHODS TO FIELD TESTING AND FACTORY SAMPLES VI-1
  (1) Introduction VI-1
  (2) Wharf Examination VI-1
  (3) Field applications of Macroanalytical Methods VI-2
  (4) Application of Macroanalytical Methods of Factory Samples VI-7
GLOSSARY G-1

Alan R. Olsen, Editor
Sherry A. Knight, Technical Editor
George C. Ziobro, Ph.D., Associate Editor

EDITORS' PREFACE

The Macroanalytical Procedures Manual is currently being revised to update its content and add new material. In the interim, we have converted the original 1984 edition of the manual for display on the FDA website. This website version was produced as a cooperative effort between the editors and the Center for Food Safety and Applied Nutrition (CFSAN). Our purpose is to provide access to the out-of-print 1984 manual until the revised edition is available.

As editors, we have tried to faithfully restore the website manuscript its original 1984 content and format. None of the methods have been changed. Where appropriate, we have inserted clearly marked editorial comments that alert users to potential changes or other useful information. In addition, we have updated (as far as possible) references to methods published by AOAC International in their compendium "Official Methods of Analysis" and to FDA Compliance Policy Guidelines.

We deeply appreciate and herein acknowledge the guidance of John C. Gecan (CFSAN) throughout the project.

We welcome any and all comments about the manual and its revision. Please address comments to the appropriate editor:

Content Editor: Alan R. Olsen, Microanalytical Entomology Specialist (Retired)
Formerly at
U.S. Food and Drug Administration
1431 Harbor Bay Parkway
Alameda, CA 94502
/ / / @ora.fda.gov

Technical Editor: Sherry A. Knight, Entomology Coordinator
U.S. Food and Drug Administration
1431 Harbor Bay Parkway
Alameda, CA 94502
sknight@ora.fda.gov

Associate and Web Editor: George C. Ziobro, Ph.D., Research Chemist (*)
U.S. Food and Drug Administration
Microanalytical Branch (HFS-315)
200 C. St. S.W.
Washington, DC 20204
gziobro@bangate.fda.gov

Electronic version 1998

* Updated contact information:
U.S. Food and Drug Administration
Division of Natural Products (HFS-315)
5100 Paint Branch Parkway
College Park, MD 20740-3835
George.Ziobro@fda.hhs.gov

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