Pesticide Analytical Manual Vol. I Chapter 1 egulatory Operations Chapter 2 General Analytical Operations and Information Chapter 3 Ch Multiclass Selective MRMS MRMS Chapter 5 GLC hapter 6 HPLC Table of contents page d 101: Regulatory Policy 101 A: Regulatory Authority 101-1 1/94 101 B: Regulatory Operations l01-21/94 101 C: Monite 101-3 1/94 Preparation of Analytical Samples 102-1 102 B: Portion of Food Commodity to be analyzed Raw Agricultural Commodities 102-1 1/94 10241/94 102 C: Compositing and Comminuting the 102-5 1/94 Laboratory sample 100
Pesticide Analytical Manual Vol. I SECTION 100 100–1 Transmittal No. 98-1 (10/97) Form FDA 2905a (6/92) Table of Contents page date 101: Regulatory Policy 101 A: Regulatory Authority 101-1 1/94 101 B: Regulatory Operations 101-2 1/94 101 C: Monitoring 101-3 1/94 References 101-3 1/94 102: Preparation of Analytical Samples 102 A: Introduction 102-1 1/94 102 B: Portion of Food Commodity to 102-1 1/94 be Analyzed Raw Agricultural Commodities 102-1 1/94 Processed Foods 102-4 1/94 102 C: Compositing and Comminuting the 102-5 1/94 Laboratory Sample Chapter 1 Regulatory Operations Chapter 2 General Analytical Operations and Information Chapter 3 Multiclass MRMs Chapter 5 GLC Chapter 4 Selective MRMs Chapter 6 HPLC
Pesticide Analytical Manual Vol I page 102 D: Handling Samples for Special Analyses 1/94 102 E: Retention of Reserve portions 1/94 References 102-6 1/94 103: Method Application in Regulatory Analysi 109 A: Introduction 1031 1/94 103 B: Choice of Method 103-11/94 PAM 103-1 1/94 Other“ Official” Method 10321/94 Other Published method 1032 1/94 103 C: Tentative Identification 103-31/94 103 D: Residue Quantitation 103-3 1/94 103 E: Confirmation of Identity 103-41/94 103 F: Documentation 1036 Analytical Reports 103- 1/94 Chromatograms 103-7 1/94 Chromatographic Data 103-71/94 103-8 1/94 104 Analytical Results 104 A: Introduction 104-1 104 B: Reporting 104-1 1/94 Portion of Commodity 104-1 Nature of the residue 10421/9 Residues measured from derivative 1/94 or Breakdown Product Significant figures 10431/94 104-3 1/94 Confirmation 104-41/94 104 C: Determining Compliance with Regulations 104-4 1/94 General Rule for Multicomponent Residues 104-4 1/94 Special Situations 104-41/94 References 104-5 1/94 105 Analytical Limits of Quantitation 105 A: Definition 105-110/97 105 B: Calculation 105-110/97 105 C: Implementation 105210/97 105 D: Factors Affecting Target Limits of Quantitation 105-2 10/97 1002 Transmit N4: 905a16/9?1
SECTION 100 Transmittal No. 98-1 (10/97) 100–2 Form FDA 2905a (6/92) Pesticide Analytical Manual Vol. I page date 102 D: Handling Samples for Special Analyses 102-6 1/94 102 E: Retention of Reserve Portions 102-6 1/94 References 102-6 1/94 103: Method Application in Regulatory Analysis 103 A: Introduction 103-1 1/94 103 B: Choice of Method 103-1 1/94 PAM 103-1 1/94 Other “Official” Methods 103-2 1/94 Other Published Methods 103-2 1/94 103 C: Tentative Identification 103-3 1/94 103 D: Residue Quantitation 103-3 1/94 103 E: Confirmation of Identity 103-4 1/94 103 F: Documentation 103-6 1/94 Analytical Reports 103-6 1/94 Chromatograms 103-7 1/94 Chromatographic Data 103-7 1/94 References 103-8 1/94 104: Analytical Results 104 A: Introduction 104-1 1/94 104 B: Reporting 104-1 1/94 Portion of Commodity 104-1 1/94 Nature of the Residue 104-2 1/94 Residues Measured from Derivative 104-2 1/94 or Breakdown Product Significant Figures 104-3 1/94 Trace 104-3 1/94 Confirmation 104-4 1/94 104 C: Determining Compliance with Regulations 104-4 1/94 General Rule for Multicomponent Residues 104-4 1/94 Special Situations 104-4 1/94 References 104-5 1/94 105: Analytical Limits of Quantitation 105 A: Definition 105-1 10/97 105 B: Calculation 105-1 10/97 105 C: Implementation 105-2 10/97 105 D: Factors Affecting Target Limits of Quantitation 105-2 10/97
Pesticide Analytical Manual Vol. I igure 102-a: Fraction of Cheese Units to Take for 1/94 Tabl 10221/94 to be analyzed for Pesticide Residues 102-b: Portion of Processed Food to be analyzed 103-a: Information Provided by Use of Element 103-51/94 Portion of Commodity for Calculation 10421/94 and Reporting of Residue levels 105-a: Examples of Method Specifications 1054 10/97 Used to Calculate L 0-3
Pesticide Analytical Manual Vol. I SECTION 100 100–3 Transmittal No. 98-1 (10/97) Form FDA 2905a (6/92) page date Figures 102-a: Fraction of Cheese Units to Take for 102-5 1/94 Compositing Tables 102-a: Portion of Raw Agricultural Commodity 102-2 1/94 to be Analyzed for Pesticide Residues 102-b: Portion of Processed Food to be Analyzed 102-4 9/96 for Pesticide Residues 103-a: Information Provided by Use of Element- 103-5 1/94 Selective Detectors 104-a: Portion of Commodity for Calculation 104-2 1/94 and Reporting of Residue Levels 105-a: Examples of Method Specifications 105-4 10/97 Used to Calculate Lqs
Pesticide Analytical Manual Vol I 100 Transmit N4: 905a16/9?1
SECTION 100 Transmittal No. 98-1 (10/97) 100–4 Form FDA 2905a (6/92) Pesticide Analytical Manual Vol. I
Pesticide Analytical Manual Vol I SECTION 101 101: REGULATORY POLICY The expressed purpose of the Pesticide Analytical Manual is to publish analytical methodology used by the FDa in enforcing pesticide tolerances. To understand FDAs application of methodology published in the manual, it is important to understand pesticide tolerance regulations and related FDA regulatory operations Material in Chapter I reflects FDA regulatory policies that affect its application of analytical methodology 101 A: REGULATORY AUTHORITY Infor n related to and the characteristics of pesticide tolerances include the follo a tolerance is the maximum concentration of a pesticide residue that is legally permitted to remain in a food. The tolerance is not expected to be exceeded if the pesticide's registered use directions are followed The statutory authority for the Environmental Protection Agencys (EPAs)establishment of tolerances is provided by sections 408 and 409 of the Federal Food, Drug, and Cosmetic Act. Tolerances established by EPA are set forth in Title 40 of the Code of federal Regulations(CFR), Part 180 for raw agricultural commodities, Part 185 for processed food, and Part 186 for animal feed. The concentration of toler- ances listed in 40 CFR 180, 185, and 186 is expressed in terms of ppm (i.e ng pesticide residue/kg food). In addition, certain pesticides are exempted from the need for tolerances; such exemptions are listed in 40 CFR 180.1001 a tolerance for a pesticide residue on a raw agricultural commodity, e.g tomatoes,also applies to processed forms of that commodity, e.g., canned tomatoes. In cases where processing may concentrate the residue, a food additive regulation may be issued in 40 CFR Part 185 to establish a higher tolerance on that processed commodity, e.g., tomato paste A tolerance regulation specifies the composition of pesticide residue for which the limit applies; i.e., a tolerance can apply to the parent form of the active ingredient only, parent compound plus one or more metabolites and/or degradation products, one or more metabolites and/or degrada- tion products only, or some chemical moiety that can be measured analyti cally for calculating the pesticide residue. a chemical entity not specified y the tolerance regulation is not included in the residue for tolerance enforcement purposes(Section 104) A tolerance regulation also specifies each individual food (e.g, apples) food group(e.g, citrus fruit) to which the limit applies No tolerance exists for a residue on a commodity unless the commodity itself or the group to which it belongs is speci In the examination of a food lot to determine whether it complies with tolerances, it is necessary to provide a sample for analysis that is represen- tative of the lot in order to determine the average pesticide residue content mittal No.94101/94 m FDA 2905a(6/92 101-1
Pesticide Analytical Manual Vol. I SECTION 101 Transmittal No. 94-1 (1/94) Form FDA 2905a (6/92) 101–1 101: REGULATORY POLICY The expressed purpose of the Pesticide Analytical Manual is to publish analytical methodology used by the FDA in enforcing pesticide tolerances. To understand FDA’s application of methodology published in the manual, it is important to understand pesticide tolerance regulations and related FDA regulatory operations. Material in Chapter 1 reflects FDA regulatory policies that affect its application of analytical methodology. 101 A: REGULATORY AUTHORITY Information related to and the characteristics of pesticide tolerances include the following: A tolerance is the maximum concentration of a pesticide residue that is legally permitted to remain in a food. The tolerance is not expected to be exceeded if the pesticide’s registered use directions are followed. The statutory authority for the Environmental Protection Agency’s (EPA’s) establishment of tolerances is provided by sections 408 and 409 of the Federal Food, Drug, and Cosmetic Act. Tolerances established by EPA are set forth in Title 40 of the Code of Federal Regulations (CFR), Part 180 for raw agricultural commodities, Part 185 for processed food, and Part 186 for animal feed. The concentration of tolerances listed in 40 CFR 180, 185, and 186 is expressed in terms of ppm (i.e., mg pesticide residue/kg food). In addition, certain pesticides are exempted from the need for tolerances; such exemptions are listed in 40 CFR 180.1001. A tolerance for a pesticide residue on a raw agricultural commodity, e.g., tomatoes, also applies to processed forms of that commodity, e.g., canned tomatoes. In cases where processing may concentrate the residue, a food additive regulation may be issued in 40 CFR Part 185 to establish a higher tolerance on that processed commodity, e.g., tomato paste. A tolerance regulation specifies the composition of pesticide residue for which the limit applies; i.e., a tolerance can apply to the parent form of the active ingredient only, parent compound plus one or more metabolites and/or degradation products, one or more metabolites and/or degradation products only, or some chemical moiety that can be measured analytically for calculating the pesticide residue. A chemical entity not specified by the tolerance regulation is not included in the residue for tolerance enforcement purposes (Section 104). A tolerance regulation also specifies each individual food (e.g., apples) or food group (e.g., citrus fruit) to which the limit applies. No tolerance exists for a residue on a commodity unless the commodity itself or the group to which it belongs is specified. In the examination of a food lot to determine whether it complies with tolerances, it is necessary to provide a sample for analysis that is representative of the lot in order to determine the average pesticide residue content