Anda di halaman 1dari 8

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STANDARD METHODS
FOR THE EXAMINATION OF

DAIRY PRODUCTS
17th Edition 2004
Edited by
H. Michael Wehr, PhD
Joseph F. Frank, PhD

American Public Health Association


800 I Street, NW
Washington, DC 20001
www.apha.org

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American Public Health Association


800 I Street, NW
Washington, DC 200013710
www.apha.org
2004 by the American Public Health Association
All rights reserved. No part of this publication may be reproduced, stored in a retrieval
system, or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, scanning, or otherwise, except as permitted under Sections 107 and
108 of the 1976 United States Copyright Act, without either the prior written permission
of the Publisher or authorization through payment of the appropriate per-copy fee to
the Copyright Clearance Center [222 Rosewood Drive, Danvers, MA 01923 (978) 7508400, fax (978) 750-4744, www.copyright.com]. Requests to the Publisher for permission
should be addressed to the Permissions Department, American Public Health Association, 800 I Street, NW, Washington, DC 20001-3710; fax (202) 777-2531.
Georges C. Benjamin, MD, FACP
Executive Director
APHA Committee on Laboratory Standards and Practices (CLaSP)
Liaison: Carl H. Blank, PhD
Printed and bound in the United States of America
Set In: Palatino and Franklin Gothic
Interior Design and Typesetting: Susan Westrate
Cover Design: Joseph R. Loehle
Printing and Binding: Victor Graphics, Inc., Baltimore, MD
ISBN 0-87553-002-8
5M 6/04

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Contents
Technical Committee . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . viii
Contributors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ix
Consensus Reviewers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xi
Preface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xiii
Chapter 1:
1.010
1.020
1.030
1.040
1.050
1.060
1.070
1.080
1.090
1.100
1.110
1.120

Chapter 2:
2.010
2.020
2.030
2.040
2.050
2.060

Chapter 3:
3.010
3.020
3.030
3.040
3.050
3.060
3.070
3.080
3.090
3.100

Chapter 4:
4.010
4.020

Standard Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
Function of Standard Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
Organization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
Changes in This Edition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
Standard Methods for International Trade . . . . . . . . . . . . . . . . . . . . . . 3
Adopting New Methodology and Uniformity of Methods . . . . . . . . 6
Classification of Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
Chapter and Method Formats Used in This Edition . . . . . . . . . . . . . . 8
Method Selection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
Split-Sample Test Program . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
Precision Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

Laboratory Quality Assurance and Safety . . . . . . . . . . . 21


Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
Quality Management System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
Quality Elements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
Common Dairy Laboratory Equipment and Supplies . . . . . . . . . . . . 38
Laboratory Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60

Sampling Dairy and Related Products . . . . . . . . . . . . . . 63


Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
Sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
Equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
General Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
Sampling Raw Milk . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 76
Sampling Pasteurized Products . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
Sampling Other Products . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81
Sampling Product Containers, Closures, Packing
Materials, Equipment, Water, and Air . . . . . . . . . . . . . . . . . . . . . . . . . 87
Radionuclides in Milk and Dairy Products (Class 0) . . . . . . . . . . . . . 90
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 90

Media and Dilution Water Preparation . . . . . . . . . . . . . . 93


Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
Suitability of Water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93

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4.030
4.040
4.050
4.060
4.070
4.080
4.090
4.100
4.110

Chapter 5:
5.010
5.020
5.030
5.040
5.050
5.060
5.070
5.080
5.090
5.100
5.110
5.120

Chapter 6:
6.010
6.020
6.030
6.040
6.050
6.060
6.070
6.080

Chapter 7:
7.010
7.020
7.030
7.040
7.050
7.060
7.070
7.080
7.090
7.100
7.110

Chapter 8:
8.010
8.020

Preparation of Dilution Water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94


Water Toxicity Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95
Cleaning Glassware and Testing for Detergent Residues . . . . . . . . . 95
Media . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
Basic Steps in Media Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
Adjustment of pH . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
Sterilization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
Quality Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100

Pathogens in Milk and Milk Products . . . . . . . . . . . . . 103


Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103
Salmonella Species Cultural Method (FDA-BAM, Class A1) . . . . . . 106
Rapid Screening Tests for Salmonella . . . . . . . . . . . . . . . . . . . . . . . . . 118
Listeria monocytogenes Cultural Method
(FDA-BAM, Class A1) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 126
Staphylococcus aureus Direct Plate Count
(FDA-BAM, Class A1) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 132
Ancillary Tests for Staphylococcus aureus . . . . . . . . . . . . . . . . . . . . . . 135
Enterotoxin Production and Isolate Analysis . . . . . . . . . . . . . . . . . . 138
Screening for Staphylococcal Enterotoxins (Class B) . . . . . . . . . . . . 138
Other Kits for Staphylococcal Enterotoxin Detection
in FoodsClass B . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 142
Mastitis Culture Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 143
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 148
Other References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 151

Microbiological Count Methods . . . . . . . . . . . . . . . . . 153


Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 153
Standard Plate Count Method (Class O) . . . . . . . . . . . . . . . . . . . . . . 154
Plate Loop Count (PLC) Method (Class 0) . . . . . . . . . . . . . . . . . . . . 168
PetrifilmTM Aerobic Plate Count (PAC) Method (Class A1) . . . . . . 174
Pectin Gel Method (Redigel) (Class A1) . . . . . . . . . . . . . . . . . . . . . . 178
Spiral Plate Count (SPLC) Method (Class A2) . . . . . . . . . . . . . . . . . 179
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 183
Other References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 185

Coliform and Other Indicator Bacteria . . . . . . . . . . . . . 187


Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 187
Colony Count Technique (without resuscitation) (Class O) . . . . . . 189
Most Probable Number Technique (Class O) . . . . . . . . . . . . . . . . . . 192
Modified VRBA Procedures (Class B) . . . . . . . . . . . . . . . . . . . . . . . . 199
Confirmed Test for Escherichia coli (Class O) . . . . . . . . . . . . . . . . . . . 199
Fluorogenic Assay (MUG Test) for Detection of
Escherichia coli in Solid Media (Class B) . . . . . . . . . . . . . . . . . . . . . . . 202
PetrifilmTM Dry Rehydratable Film Methods . . . . . . . . . . . . . . . . . . 203
Pectin Gel Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 215
Enterobacteriaceae . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 221
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 224
Other References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 226

Tests for Groups of Microorganisms . . . . . . . . . . . . . . 227


Psychrotrophic Bacteria (Class O) . . . . . . . . . . . . . . . . . . . . . . . . . . . 227
Gram-Negative Bacteria (Class B) . . . . . . . . . . . . . . . . . . . . . . . . . . . 228

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8.030
8.040
8.050
8.060
8.070
8.080
8.090
8.100
8.110
8.120

Chapter 9:
9.010
9.020
9.030
9.040
9.050
9.060
9.070
9.080
9.090
9.100
9.110

Chapter 10:
10.010
10.020
10.030
10.040

Chapter 11:
11.010
11.020
11.030
11.040
11.050
11.060

Chapter 12:
12.010
12.020
12.030
12.040
12.050
12.060
12.070
12.080
12.090
12.100
12.110

Thermoduric Bacteria (Class O) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 229


Thermophilic Bacteria (Class O) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 230
Proteolytic Microorganisms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 231
Lipolytic Microorganisms (Class B) . . . . . . . . . . . . . . . . . . . . . . . . . . 233
Lactic Acid Bacteria (Class B) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 235
Enterococci (Class B) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 237
Aerobic Bacterial Spores (Class B) . . . . . . . . . . . . . . . . . . . . . . . . . . . 239
Anaerobic Sporeformers (Class B) . . . . . . . . . . . . . . . . . . . . . . . . . . . 240
Yeast and Mold Counts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 242
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 246

Microbiological Methods for Dairy Products . . . . . . . . . 249


Fluid Milk Products: Shelf Life . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 249
Preliminary Incubation Method for Processed
Milk Products (Class B) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 251
Concentrated Milk Products . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 252
Ultra-High-Temperature Processed, Aseptically
Packaged, Low-Acid Products (Class B) . . . . . . . . . . . . . . . . . . . . . . 254
Dairy Products . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 255
Butter, Margarine, and Related Products . . . . . . . . . . . . . . . . . . . . . 257
Cheese . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 258
Yogurt and Other Fermented Milk Products . . . . . . . . . . . . . . . . . . 261
Ice Cream and Related Food Products . . . . . . . . . . . . . . . . . . . . . . . 263
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 265
Other References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 265

Direct Microscopic Methods for Bacteria


or Somatic Cells . . . . . . . . . . . . . . . . . . . . . . . . . . . . 269
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 269
Direct Microscopic Count . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 270
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 279
Other References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 280

Methods to Detect Abnormal Milk . . . . . . . . . . . . . . . 281


Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 281
Cowside Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 281
Laboratory Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 285
Laboratory Tests to Detect Abnormal Goats Milk . . . . . . . . . . . . . . 289
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 290
Other References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 292

Detection of Antibiotic/Drug Residues in


Milk and Dairy Products . . . . . . . . . . . . . . . . . . . . . . 293
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 293
Growth Inhibition Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 294
Enzyme Substrate TestsBeta Lactam Specific . . . . . . . . . . . . . . . . 302
Receptor Assay TestsBeta Lactam Specific . . . . . . . . . . . . . . . . . . 305
ELISA TestsBeta Lactam Specific . . . . . . . . . . . . . . . . . . . . . . . . . . 312
Sulfonamide Assays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 316
Tetracycline Assays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 318
Chloramphenicol Assays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 320
High-Performance Liquid Chromatography (HPLC) . . . . . . . . . . . 321
Assays for Other Inhibitors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 322
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 322

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Chapter 13:
13.010
13.020
13.030
13.040
13.050

Chapter 14:
14.010
14.020
14.030
14.040
14.050
14.060
14.070
14.080

Chapter 15:
15.010
15.020
15.030
15.040
15.050
15.060
15.070
15.080
15.090
15.100
15.110
15.120
15.130
15.140
15.150
15.160
15.170
15.180

Chapter 16:
16.010
16.020
16.030
16.040
16.050
16.060

Microbiological Tests for Equipment,


Containers, Water, and Air . . . . . . . . . . . . . . . . . . . . . 325
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 325
Tests for the Microbiological Quality of Air . . . . . . . . . . . . . . . . . . . 325
Tests for Water Supplies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 328
Tests for Equipment and Containers . . . . . . . . . . . . . . . . . . . . . . . . . 328
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 338

Alkaline Phosphatase Methods . . . . . . . . . . . . . . . . . 341


Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 341
Scharer Rapid Visual ALP Method (Class O) . . . . . . . . . . . . . . . . . . 344
Scharer Spectrophotometric ALP Method . . . . . . . . . . . . . . . . . . . . 351
Rutgers Visual ALP Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 353
Fluorophos Fluorometric ALP Method . . . . . . . . . . . . . . . . . . . . . . 355
Charm Chemiluminescent ALP Method (Class A1) . . . . . . . . . . . . . 358
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 361
Other References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 362

Chemical and Physical Methods . . . . . . . . . . . . . . . . . 363


Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 363
Acidity Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 363
Adulterant Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 374
Ash Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 380
Chloride Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 385
Contaminant Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 391
Extraneous Material Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 403
Fat Determination Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 408
Lactose and Galactose Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 434
Minerals and Food Additives . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 440
Moisture and Solids Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 442
Multicomponent Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 460
Protein/Nitrogen Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 480
Rancidity Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .510
Sanitizer Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 514
Vitamins A, D2, and D3 in Milk Products, HPLC
Method (Class O) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 519
Functional Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 527
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 532

Milk and Milk Products Standards

. . . . . . . . . . . . . . .537

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 537
Nutrition and Labeling Requirements . . . . . . . . . . . . . . . . . . . . . . . . 537
Compositional Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 540
International Compositional Specifications . . . . . . . . . . . . . . . . . . . . 546
Microbiological Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548
Cited References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 550

Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .551

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DEDICATION
Carl H. Blank, PhD
March 16, 1927 May 4, 2002

Dedicated to the memory of Carl H. Blank, PhD, a member of the


American Public Health Association for over 40 years; former chair of
APHA's Laboratory Section (19771978); a long time member and former
chair of APHA's Committee on Laboratory Standards and Practices
(CLaSP); and CLaSP liaison to the Technical Committee for this 17th edition of Standard Methods for the Examination of Dairy Products.

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Technical Committee
H. Michael Wehr, PhD, Chair
U.S. Food and Drug Administration
Washington, DC 20204
Edward A. Arnold, Jr.
Land O'Lakes/R. Tech Laboratories, Inc.
Arden Hills, MN 55126
Mary Bulthaus
Dairy Quality Control Institute
Moundsview, MN 551121400
John C. Bruhn, PhD
Department of Food Science and Technology
University of California
Davis, CA 956168598
James E. Fitts
Division of Milk Control
New York Department of Agriculture and Markets
Albany, NY 12235
Joseph F. Frank, PhD
Department of Food Science and Technology
University of Georgia
Athens, GA 306027610
Robert T. Marshall, PhD
Department of Food Science and Nutrition
University of Missouri
Columbia, MO 65211
Larry A. Maturin, PhD
U.S. Food and Drug Administration
Laboratory Quality Assurance Branch
Summit Argo, IL 605011957
APHA Committee on Laboratory Science and Practice (CLaSP) Liaison
Carl H. Blank, PhD
APHA Project Liaison
Ellen T. Meyer
Director of Publications