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