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
SECTION 101 Pesticide Analytical Manual Vol I of the lot. Tolerances apply to that sample or a representative portion of Unless otherwise specified in a tolerance regulation, each tolerance ap- lies to the whole portion of a food commodity that moves in commerce n practice, however, some food commodities(mainly raw agricultural commodities) require further definition as to the portion of commodity to which a tolerance applies and which is to be analyzed In summary, a tolerance provides a means of ascertaining that a pesticide was properly used. If a pesticide residue is found to exceed a tolerance or be present in a food for which there is no tolerance, then the pesticide was not used in a manner consistent with the tolerance. Under Sections 402(a)(2)(B)or(C)of the Federal Food, Drug, and Cosmetic Act, this constitutes a violation of the law; i.e., the food commodity is adulterated because it contains an"unsafe"or illegal ticide residue 101 B: REGULATORY OPERATIONS To fulfill its responsibility to enforce regulations on pesticide residues in foods, FDA maintains a comprehensive pesticide program, including the analysis of food for enforcement of pesticide tolerances. Although the majority of samples ana- lyzed contain no violative residues, sample handling must be consistent for all analyzed samples, because it is impossible to know in advance which samples will contain violative residues Accordingly, the following procedures must be followed by FDA laboratories to establish that a product contains illegal pesticide residue(s) 1)A laboratory sample of food must be collected from a consignment accordance with agency sample collection instructions [1]; this laboratory sample is then considered representative of the food consignment. 2)The portion of food taken from the laboratory sample (whole product or specified parts of product) must be in accordance with agency instructions, and that portion must be appropriately composited and com- minuted (Section 102). From that resulting test sample, a test portion is taken for analysis; test portion size is dictated by requirements of the analytical method. Residues found in the test portion are considered rep resentative of the average residue content of the original consignment related to food products in this chapte signment, "laboratory sample, " test sample, te rtion reflects rec ommendations of IUPAC Analytical Chemistry n. Commission on Analytical Nomenclature [2]. Common usage, however, usually refers to the test portion as"sample, and this convention is used throughout most f PAM I. 3)The test portion must be analyzed by a published, official analytical method or one that has been validated for the specific pesticide /commodity por nd findings of residues must be confirmed (Section 108). For FDa monitoring purposes, analytical methods must be capable of accurately 101- Transmittal No. 94-1(1/941 Form FDA 2905a(6/92
SECTION 101 Pesticide Analytical Manual Vol. I 101–2 Transmittal No. 94-1 (1/94) Form FDA 2905a (6/92) of the lot. Tolerances apply to that sample or a representative portion of that sample. Unless otherwise specified in a tolerance regulation, each tolerance applies to the whole portion of a food commodity that moves in commerce. In practice, however, some food commodities (mainly raw agricultural commodities) require further definition as to the portion of commodity to which a tolerance applies and which is to be analyzed. In summary, a tolerance provides a means of ascertaining that a pesticide was properly used. If a pesticide residue is found to exceed a tolerance or be present in a food for which there is no tolerance, then the pesticide was not used in a manner consistent with the tolerance. Under Sections 402 (a) (2) (B) or (C) of the Federal Food, Drug, and Cosmetic Act, this constitutes a violation of the law; i.e., the food commodity is adulterated because it contains an “unsafe” or illegal pesticide residue. 101 B: REGULATORY OPERATIONS To fulfill its responsibility to enforce regulations on pesticide residues in foods, FDA maintains a comprehensive pesticide program, including the analysis of food for enforcement of pesticide tolerances. Although the majority of samples analyzed contain no violative residues, sample handling must be consistent for all analyzed samples, because it is impossible to know in advance which samples will contain violative residues. Accordingly, the following procedures must be followed by FDA laboratories to establish that a product contains illegal pesticide residue(s): 1) A laboratory sample of food must be collected from a consignment in accordance with agency sample collection instructions [1]; this laboratory sample is then considered representative of the food consignment. 2) The portion of food taken from the laboratory sample (whole product or specified parts of product) must be in accordance with agency instructions, and that portion must be appropriately composited and comminuted (Section 102). From that resulting test sample, a test portion is taken for analysis; test portion size is dictated by requirements of the analytical method. Residues found in the test portion are considered representative of the average residue content of the original consignment. (Note that terminology related to food products in this chapter, i.e., “consignment,” “laboratory sample,” “test sample,” “test portion,” reflects recommendations of IUPAC Analytical Chemistry Division, Commission on Analytical Nomenclature [2]. Common usage, however, usually refers to the test portion as “sample,” and this convention is used throughout most of PAM I.) 3) The test portion must be analyzed by a published, official analytical method or one that has been validated for the specific pesticide/commodity portion, and findings of residues must be confirmed (Section 103). For FDA monitoring purposes, analytical methods must be capable of accurately
Pesticide Analytical Manual Vol I SECTION 101 measuring pesticide residues as defined by the tolerance regulation at not only the tolerance limit but also the lower limit of quantitation (Section 105) 4)If the residue level found in the original analysis exceeds an established tolerance, or if no tolerance exists for the residue in that commodity, another analysis of a second test portion of the same composited test sample must be conducted by a second analyst(normally a senior ana- yst); the second analysis is referred to as a"check analysis 5)If check analysis verifies that the residue violates a regulation, i.e., the results of both original and check analyses exceed a tolerance and are in close agreement or are in close agreement for pesticide residues for which there is no tolerance, the analytical findings will support enforce- ment action against the food consignment. If the check analysis result is below a tolerance or if the results of the original and check analyses are widely divergent, enforcement action cannot be supported. Addi- tional analyses may be required to resolve widely divergent analytical 101C. MONITORING The FDA pesticide program has two main objectives: (1)to enforce residue toler ances and(2)to determine incid and level of residues in the food supply. The section above defines operations established to enforce regulations Monitoring aspects of the programs can be accomplished simultaneously, because levels of all residues found are calculated and recorded, whether or not they support enforcement action. Section 104 provides information about reportin residues for monitoring purposes, as well as determining compliance with regula- tions References [1] Investigations Operation Manual, Sample Schedule Chart 3, FDA, Rockville, MD [2] Horwitz, W.(1990) Pure Appl. Chem. 62, 1199-1208 m FDA 2905a(6/92 101-3
Pesticide Analytical Manual Vol. I SECTION 101 Transmittal No. 94-1 (1/94) Form FDA 2905a (6/92) 101–3 measuring pesticide residues as defined by the tolerance regulation at not only the tolerance limit but also the lower limit of quantitation (Section 105). 4) If the residue level found in the original analysis exceeds an established tolerance, or if no tolerance exists for the residue in that commodity, another analysis of a second test portion of the same composited test sample must be conducted by a second analyst (normally a senior analyst); the second analysis is referred to as a “check analysis.” 5) If check analysis verifies that the residue violates a regulation, i.e., the results of both original and check analyses exceed a tolerance and are in close agreement or are in close agreement for pesticide residues for which there is no tolerance, the analytical findings will support enforcement action against the food consignment. If the check analysis result is below a tolerance or if the results of the original and check analyses are widely divergent, enforcement action cannot be supported. Additional analyses may be required to resolve widely divergent analytical results. 101 C: MONITORING The FDA pesticide program has two main objectives: (1) to enforce residue tolerances and (2) to determine incidence and level of pesticide residues in the food supply. The section above defines operations established to enforce regulations. Monitoring aspects of the programs can be accomplished simultaneously, because levels of all residues found are calculated and recorded, whether or not they support enforcement action. Section 104 provides information about reporting residues for monitoring purposes, as well as determining compliance with regulations. References [1] Investigations Operation Manual, Sample Schedule Chart 3, FDA, Rockville, MD [2] Horwitz, W. (1990) Pure Appl. Chem. 62, 1193-1208
SECTION 101 Pesticide Analytical Manual Vol I 101-4 Transmittal No. 94-1(1/941 Form FDA 2905a(6/92
SECTION 101 Pesticide Analytical Manual Vol. I 101–4 Transmittal No. 94-1 (1/94) Form FDA 2905a (6/92)
Pesticide Analytical Manual Vol. I SECTION 102 102: PREPARATION OF ANALYTICAL SAMPLES 102 A: INTRODUCTION This section contains directions for preparation of test samples of food from labo- ratory samples collected for pesticide residue analysis. The following topics are considered, but not all are pertinent to every sample situation: (1)instructions for portion of commodity to be analyzed for pesticide residues,(2)directions for compositing and comminuting food items, ( 3)procedures for samples that are to undergo special analyses, and(4)requirements for retention of reserve portions of test samples 102 B: PORT/ON OF FOOD COMMODITY TO BE ANALYZED As a general approach, the"portion of commodity"composited to create the test sample consists of the entire food commodity(e.g, whole cantaloupe). For many raw and processed foods, however, only specific portions of the food are included in the composite for the test sample to ensure uniformity and consistency in tolerance enforcement and related monitoring, it is necessary to adhere to the following instructions on the portion of comm odity to be analyzed Raw Agricultural Commodities EPA regulations [1] specify that a raw agricultural commodity examined for com- pliance with a pesticide tolerance consist of the " whole raw agricultural commod- ity. The regulations contain some specific instructions on what constitutes the hole raw agricultural commodity; e.g,"caps(hulls) shall be removed and dis- carded from strawberries before examination for pesticide residues. " Such instruc- tions are provided for only nine individual food commodities(e.g, bananas) and crop group commodities (e.g, root vegetables) Recognizing the limitation of these regulations, FDA developed directions for additional commodities, taking into account practical considerations of sample preparation (e.g, removal of stones from peaches to facilitate preparation of a homogenate). Table 102-a is a compilation of EPA regulations and FDa direc- tions(An EPA rulemaking is expected to be initiated that would amend the above existing regulation to incorporate FDA's more complete instructions on the por tion of commodity to which a tolerance applies and that is to be analyzed.) In some instances, a pesticide tolerance regulation specifies an exception to direc- tions in Table 102-a. For example, the tolerance for mevinphos residues on mel- ons states that compliance with the tolerance is to be "determined on the edible portion with rind removed, [2] even though the tolerances for most other pes- ticides on melons apply to the whole commodity including the rind. Follow these directions to prepare test samples of raw agricultural commodities Use the entire raw agricultural commodity, as specified in Table 102-a. When a pesticide residue is found in a commodity for which the tolerance applies to a portion different from that specified in Table 102-a, prepare a new test sample in accordance with the pesticide's tolerance regulation. mittal No.94101/94 m FDA 2905a(6/92 102-1
SECTION 102 102–1 Transmittal No. 94-1 (1/94) Form FDA 2905a (6/92) Pesticide Analytical Manual Vol. I 102: PREPARATION OF ANALYTICAL SAMPLES 102 A: INTRODUCTION This section contains directions for preparation of test samples of food from laboratory samples collected for pesticide residue analysis. The following topics are considered, but not all are pertinent to every sample situation: (1) instructions for portion of commodity to be analyzed for pesticide residues, (2) directions for compositing and comminuting food items, (3) procedures for samples that are to undergo special analyses, and (4) requirements for retention of reserve portions of test samples. 102 B: PORTION OF FOOD COMMODITY TO BE ANALYZED As a general approach, the “portion of commodity” composited to create the test sample consists of the entire food commodity (e.g., whole cantaloupe). For many raw and processed foods, however, only specific portions of the food are included in the composite for the test sample. To ensure uniformity and consistency in tolerance enforcement and related monitoring, it is necessary to adhere to the following instructions on the portion of commodity to be analyzed. Raw Agricultural Commodities EPA regulations [1] specify that a raw agricultural commodity examined for compliance with a pesticide tolerance consist of the “whole raw agricultural commodity.” The regulations contain some specific instructions on what constitutes the whole raw agricultural commodity; e.g., “caps (hulls) shall be removed and discarded from strawberries before examination for pesticide residues.” Such instructions are provided for only nine individual food commodities (e.g., bananas) and crop group commodities (e.g., root vegetables). Recognizing the limitation of these regulations, FDA developed directions for additional commodities, taking into account practical considerations of sample preparation (e.g., removal of stones from peaches to facilitate preparation of a homogenate). Table 102-a is a compilation of EPA regulations and FDA directions. (An EPA rulemaking is expected to be initiated that would amend the above existing regulation to incorporate FDA’s more complete instructions on the portion of commodity to which a tolerance applies and that is to be analyzed.) In some instances, a pesticide tolerance regulation specifies an exception to directions in Table 102-a. For example, the tolerance for mevinphos residues on melons states that compliance with the tolerance is to be “determined on the edible portion with rind removed,” [2] even though the tolerances for most other pesticides on melons apply to the whole commodity including the rind. Follow these directions to prepare test samples of raw agricultural commodities: • Use the entire raw agricultural commodity, as specified in Table 102-a. • When a pesticide residue is found in a commodity for which the tolerance applies to a portion different from that specified in Table 102-a, prepare a new test sample in accordance with the pesticide’s tolerance regulation
SECTION 102 Pesticide Analytical Manual Vol I Table 102-a: Portion of Raw Agricultural Commodity to be Analyzed for Pesticide Residues Root and tuber vegetables group Where separate tolerances are established for root or tuber, analyze whole commodity after removing adhering soil by lightly rinsing in running wate Where a tolerance is established on a root veg. etable including tops andy or with tops, and tops and roots are marketed together, analyze tops and roots separately. Neither the pesticide residue on the roots nor the pesticide residue on the top shall exceed the tolerance level for carrots parsnips, and rutabagas, remove and discard tops Bulb vegetables(green or dry) Whole commodity after removing and discarding group roots. Remove adhering soil by lightly rinsing in running water. In the case of dry bulb onions and garlic, remove and discard stems and outer sheaths (husk or parchment skin) that are easily removed Leafy vegetables(except Whole commodity after removing and discarding Brassica vegetables) group obviously decomposed or withered leaves. In the case of rhubarb, analyze only the stem without leaves. Remove adhering soil from celery by lightly rinsing In running water obviously decomposed or withe, g and discarding Brassica(cole) leafy vegetables Whole commodity after removin group ed leaves, except remove and discard all leaves from cauliflower and headed broccoli and use sprouts only from brussels sprouts egume vegetables(succulent Whole commodity, including pods for succulent and or dried) group without pods for dry Fruiting vegetables(except Whole commodity after removing and discarding cucurbits)group stems and husk Cucurbit vegetables group Whole commodity after removing and discarding Citrus fruits Whole commodity Pome fruits group Whole commodity after removing and discarding stems Stone fruits group Whole commodity after removing and discarding Small fruits and berries group Whole commodity after removing and discarding caps and stems, except for currants, where the stems are to be included I Members of food groups are listed in 40 CFR 180.34(6)(9) 102-2 Transmittal No. 94-1(1/941 Form FDA 2905a(6/92
Transmittal No. 94-1 (1/94) 102–2 Form FDA 2905a (6/92) SECTION 102 Pesticide Analytical Manual Vol. I 1 Members of food groups are listed in 40 CFR 180.34 (f)(9). Table 102-a: Portion of Raw Agricultural Commodity to be Analyzed for Pesticide Residues Root and tuber vegetables group1 Where separate tolerances are established for root or tuber, analyze whole commodity after removing adhering soil by lightly rinsing in running water. Where a tolerance is established on a root vegetable including tops and/or with tops, and tops and roots are marketed together, analyze tops and roots separately. Neither the pesticide residue on the roots nor the pesticide residue on the tops shall exceed the tolerance level. For carrots, parsnips, and rutabagas, remove and discard tops. Bulb vegetables (green or dry) Whole commodity after removing and discarding group roots. Remove adhering soil by lightly rinsing in running water. In the case of dry bulb onions and garlic, remove and discard stems and outer sheaths (husk or parchment skin) that are easily removed. Leafy vegetables (except Whole commodity after removing and discarding Brassica vegetables) group obviously decomposed or withered leaves. In the case of rhubarb, analyze only the stem without leaves. Remove adhering soil from celery by lightly rinsing in running water. Brassica (cole) leafy vegetables Whole commodity after removing and discarding group obviously decomposed or withered leaves, except remove and discard all leaves from cauliflower and headed broccoli and use sprouts only from brussels sprouts. Legume vegetables (succulent Whole commodity, including pods for succulent and or dried) group without pods for dry. Fruiting vegetables (except Whole commodity after removing and discarding cucurbits) group stems and husks. Cucurbit vegetables group Whole commodity after removing and discarding stems. Citrus fruits group Whole commodity. Pome fruits group Whole commodity after removing and discarding stems. Stone fruits group Whole commodity after removing and discarding stems and stones. Small fruits and berries group Whole commodity after removing and discarding caps and stems, except for currants, where the stems are to be included
