《美国FDA农残分析手册》（第一卷英文版）VOLUME Multiresidue methods

PESTICIDE NALY TICAL MANUAL VOLUME Multiresidue methods F△ Z.S. Department of Health and Human Services Public Health Service Food and Drug administration

MANUAL VOLUME I: Multiresidue Methods U.S. Department of Health and Human Services • Public Health Service Food and Drug Administration PESTICIDE ANALY TICAL RAPE D MT ENT OF HEALTH & HUMAN SERVICES . USA

Pesticide Analytical Manual Vol I PESTICIDE ANALYTICAL MANUAL VOLUME I 3rd edition 1994 Revised, September, 1996 Revised. October. 1997 Revised. October 1999 EDITORIAL STAFF Carolyn M. Makovi, Editor Bernadette M. Mcmahon. Editor emerita EDITORIAL BOARD Marion Clower, ]r, Ph D Charles H. Parfitt, Jr. JohnJ O Rangers, Jr, Ph D Ronald R. roy Richard Schmitt. Ph. D. ePA TECHNICAL ADVISORS Jerry E Froberg Marvin L Hopper Fred r. Krick Ronald G. Luchtefeld Milton a. Luke MANAGING EDITORS Management Methods Branch Office of the Associate Commissioner for Management and Operatic Design and Format: R.O. w. Sciences, Inc. under contract to U.S. Food and drug administration The mention of specific items of equipment and chemicals by brand name or the supplying of manufacturers names and addresses do not constitute endorsement of a product or source by the United States Government. Form FDA 2905a(6

Pesticide Analytical Manual Vol. I Transmittal No. 2000-1 (10/1999) Form FDA 2905a (6/92) PESTICIDE ANALYTICAL MANUAL VOLUME I 3rd Edition, 1994 Revised, September, 1996 Revised, October, 1997 Revised, October 1999 EDITORIAL STAFF Carolyn M. Makovi, Editor Bernadette M. McMahon, Editor Emerita EDITORIAL BOARD Marion Clower, Jr., Ph.D. Charles H. Parfitt, Jr. John J. O’Rangers, Jr., Ph.D. Ronald R. Roy Richard Schmitt, Ph.D., EPA TECHNICAL ADVISORS Jerry E. Froberg Marvin L. Hopper Fred R. Krick Ronald G. Luchtefeld Milton A. Luke MANAGING EDITORS Management Methods Branch Office of the Associate Commissioner for Management and Operations Design and Format: R.O.W. Sciences, Inc. under contract to U.S. Food and Drug Administration The mention of specific items of equipment and chemicals by brand name or the supplying of manufacturers’ names and addresses do not constitute endorsement of a product or source by the United States Government

Pesticide Analytical Manual Vol. I TABLE OF CONTENTS PESTICIDE ANALYTICAL MANUAL VOLUME I TABLE OF CONTENTS Introduction to pam Preface to pam i 3rd edition Guide to use of pami Chapter l Regulatory Operations 102 Preparation of Analytical Samples 103 Method Application in Regulatory analy 104 Analytical Results 105 Analytical Limits of Quantitation Chapter 2 General Analytical Operations and Information 201 Percentage Fat, Water, and Sugars in Foods 202 Basic Analytical Techniques 203 Equipment and Procedures for Comminuting 204 Special Reagent Preparation 206 Quality Assurance/Quality Control 207 Laboratory Safety 208 Hazardous Waste Disposal Chapter 3 Multiclass Multiresidue Methods 801 General Information 302 Method I for Nonfatty Foods 303 Method II for Nonfatty Foods 304 Method for Fatty Foods Chapter 4 Selective Multiresidue Methods 0l Method for N-Methylcarbamates 402 Method for Acids and phenols 403 Method for Phenylurea Herbicides 404 Method for benzimidazoles

Pesticide Analytical Manual Vol. I TABLE OF CONTENTS iii Transmittal No. 94-1 (1/94) Form FDA 2905a (6/92) PESTICIDE ANALYTICAL MANUAL VOLUME I TABLE OF CONTENTS Introduction to PAM Preface to PAM I 3rd edition Guide to Use of PAM I Chapter 1 Regulatory Operations 101 Regulatory Policy 102 Preparation of Analytical Samples 103 Method Application in Regulatory Analysis 104 Analytical Results 105 Analytical Limits of Quantitation Chapter 2 General Analytical Operations and Information 201 Percentage Fat, Water, and Sugars in Foods 202 Basic Analytical Techniques 203 Equipment and Procedures for Comminuting 204 Special Reagent Preparation 205 Reference Standards 206 Quality Assurance/Quality Control 207 Laboratory Safety 208 Hazardous Waste Disposal Chapter 3 Multiclass Multiresidue Methods 301 General Information 302 Method I for Nonfatty Foods 303 Method II for Nonfatty Foods 304 Method for Fatty Foods Chapter 4 Selective Multiresidue Methods 401 Method for N-Methylcarbamates 402 Method for Acids and Phenols 403 Method for Phenylurea Herbicides 404 Method for Benzimidazoles

TABLE OF CONTENTS Pesticide Analytical Manual Vol I Chapter 5 Gas Liquid Chromatography 01 General Information 502 Columns 503 Detectors 504 Quantitation 05 Bibliography Chapter 6 High Performance Liquid Chromatography 601 General Information 602 Columns 603 Mobile Phase Selection, Preparation, and Delivery 604 Injection Systems 605 Detectors 606 Residue Identification and Quantitation 607 Quality Assurance and Troubleshooting 608 Bibliography Appendix I PESTDATA Appendix II Protocols and Reporting Forms for Testing Chemicals Through PAM multiresidue methods Index to PAM I Methods, by Chemicals Tested for Recovery Index to Names used for Chemicals in Pami Index to CAS Registry Numbers for Chemicals in PAM I Index to Subjects Transmittal No. 94-1(1/94] Form FDA 2905a(6/92]

TABLE OF CONTENTS Pesticide Analytical Manual Vol. I Transmittal No. 94-1 (1/94) iv Form FDA 2905a (6/92) Chapter 5 Gas Liquid Chromatography 501 General Information 502 Columns 503 Detectors 504 Quantitation 505 Bibliography Chapter 6 High Performance Liquid Chromatography 601 General Information 602 Columns 603 Mobile Phase Selection, Preparation, and Delivery 604 Injection Systems 605 Detectors 606 Residue Identification and Quantitation 607 Quality Assurance and Troubleshooting 608 Bibliography Appendix I PESTDATA Appendix II Protocols and Reporting Forms for Testing Chemicals Through PAM Multiresidue Methods Index to PAM I Methods, by Chemicals Tested for Recovery Index to Names Used for Chemicals in PAM I Index to CAS Registry Numbers for Chemicals in PAM I Index to Subjects

Pesticide Analytical Manual Vol. I INTRODUCTION PESTICIDE ANALYTICAL MANUAL INTRODUCTION The Food and Drug Administration(FDA) is responsible under the Federal Food Drug, and Cosmetic Act for enforcing tolerances established by the environmental Protection Agency(EPA) for amounts of pesticide residues that may legally re- main on food(including animal feed). In meeting this responsibility, FDA collects and analyzes food from commercial channels of trade for determining compliance with EPA tolerances. The residue data gathered under this regulatory monitoring program are also used for evaluating the extent and significance of pesticide residues in the food supply The Pesticide Analytical Manual(PAM) is published by FDA as a repository of the analytical methods used in FDA laboratories to examine food for pesticide resi- dues for regulatory purposes. The manual is organized according to the scope of the analytical methods Volume i contains multiresidue methods (MRMs) that are used by FDa on a routine basis, because of their efficiency and broad applicability especially for analyzing foods of unknown pesticide treatment his- Volume ii contains methods designed for the analysis of commodities for resi- dues of only a single compound (although some methods are ca- pable of determining several related compounds). These methods are most often used when the likely residue is known to the chemist and/or when the residue of interest cannot be determined by com- mon mrms PAM is designed to be used by analysts experienced in trace residue analysis. All of the techniques employed are subject to potential interferences from reagents apparatus, containers, contaminated air supply, and handling by personnel. The experienced analyst is alert for these possibilities and recognizes the need to con- firm results by other techniques that measure different chemical or physical prop erties of the analyte Expe particular application by a trial of the method that includes examination of re- editors invite analysts to report results of their experiences with PAM methode agent and sample blanks and measurement of the recovery of added analyte. the Revisions Starting with transmittal 96-1(9/96), revisions of PAM I have been issued in two ways (1) changes in most manual sections will be distributed as hard(paper)copies, with symbols or marking lines that have been changed, and(2)updates to the tables 140CFR180.101(c) Form FDA 2905a(6/92)

Transmittal No. 98-1 (10/97) Form FDA 2905a (6/92) v Pesticide Analytical Manual Vol. I PESTICIDE ANALYTICAL MANUAL INTRODUCTION The Food and Drug Administration (FDA) is responsible under the Federal Food, Drug, and Cosmetic Act for enforcing tolerances established by the Environmental Protection Agency (EPA) for amounts of pesticide residues that may legally re￾main on food (including animal feed). In meeting this responsibility, FDA collects and analyzes food from commercial channels of trade for determining compliance with EPA tolerances. The residue data gathered under this regulatory monitoring program are also used for evaluating the extent and significance of pesticide residues in the food supply. The Pesticide Analytical Manual (PAM) is published by FDA as a repository of the analytical methods used in FDA laboratories to examine food for pesticide resi￾dues for regulatory purposes.1 The manual is organized according to the scope of the analytical methods: Volume␣ I contains multiresidue methods (MRMs) that are used by FDA on a routine basis, because of their efficiency and broad applicability, especially for analyzing foods of unknown pesticide treatment his￾tory. Volume II contains methods designed for the analysis of commodities for resi￾dues of only a single compound (although some methods are ca￾pable of determining several related compounds). These methods are most often used when the likely residue is known to the chemist and/or when the residue of interest cannot be determined by com￾mon MRMs. PAM is designed to be used by analysts experienced in trace residue analysis. All of the techniques employed are subject to potential interferences from reagents, apparatus, containers, contaminated air supply, and handling by personnel. The experienced analyst is alert for these possibilities and recognizes the need to con￾firm results by other techniques that measure different chemical or physical prop￾erties of the analyte. Experienced residue analysts are aware that no report of validation in another laboratory can substitute for verification that the method does indeed work in the analyst’s own laboratory. The analyst should verify method performance in each particular application by a trial of the method that includes examination of re￾agent and sample blanks and measurement of the recovery of added analyte. The editors invite analysts to report results of their experiences with PAM methods. Revisions Starting with transmittal 96-1 (9/96), revisions of PAM I have been issued in two ways: (1) changes in most manual sections will be distributed as hard (paper) copies, with symbols or marking lines that have been changed, and (2) updates to the tables 1 40 CFR 180.101 (c) INTRODUCTION