CACGL 33-1999 Recommended Methods of Sampling for Pesticide Residues for the Determination of Compl.pdf
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1、CAC/GL 33 Page 1 of 20 RECOMMENDED METHODS OF SAMPLING FOR THE DETERMINATION OF PESTICIDE RESIDUES FOR COMPLIANCE WITH MRLS CAC/GL 33-1999 CONTENTS Pages OBJECTIVE.1 PRINCIPLES1 SAMPLING PROCEDURES.2 CRITERIA FOR DETERMINING COMPLIANCE .3 TABLE 1. MINIMUM NUMBER OF PRIMARY SAMPLES TO BE TAKEN FROM A
2、 LOT4 (a) Meat and poultry.4 (b) Other products.4 TABLE 2. NUMBER OF RANDOMLY SELECTED PRIMARY SAMPLES REQUIRED FOR A GIVEN PROBABILITY OF FINDING AT LEAST ONE NON-COMPLIANT SAMPLE IN A LOT OF MEAT OR POULTRY, FOR A GIVEN INCIDENCE OF NON-COMPLIANT RESIDUES IN THE LOT5 TABLE 3. MEAT AND POULTRY PROD
3、UCTS: DESCRIPTION OF PRIMARY SAMPLES AND MINIMUM SIZE OF LABORATORY SAMPLES 6 TABLE 4. PLANT PRODUCTS: DESCRIPTION OF PRIMARY SAMPLES AND MINIMUM SIZE OF LABORATORY SAMPLES9 TABLE 5. EGG AND DAIRY PRODUCTS: DESCRIPTION OF PRIMARY SAMPLES AND MINIMUM SIZE OF LABORATORY SAMPLES11 ANNEX I. DEFINITION O
4、F TERMS.13 ANNEX II.A SCHEMATIC REPRESENTATION OF SAMPLING: MEAT AND POULTRY.17 ANNEX II.B SCHEMATIC REPRESENTATION OF SAMPLING: PRODUCTS OTHER THAN MEAT AND POULTRY .18 ANNEX III. EXAMPLES.19 REFERENCES.20 RECOMMENDED METHODS OF SAMPLING FOR THE DETERMINATION OF PESTICIDE RESIDUES FOR COMPLIANCE WI
5、TH MRLS 1. OBJECTIVE The objective of these sampling procedures is to enable a representative sample to be obtained from a lot, for analysis to determine compliance with Codex Maximum Residue Limits (MRLs) for pesticides. 2. PRINCIPLES 2.1 Codex MRLs are based on Good Agricultural Practice data and
6、foods derived from commodities that comply with the respective Codex MRLs are intended to be toxicologically acceptable. 2.2 A Codex MRL for a plant, egg or dairy product takes into account the maximum level expected to occur in a composite sample, which has been derived from multiple units of the t
7、reated product and which is intended to represent the average residue level in a lot. A Codex MRL for meat and poultry takes into account the maximum level expected to occur in the tissues of individual treated animals or birds. CAC/GL 33 Page 2 of 20 2.3 In consequence, MRLs for meat and poultry ap
8、ply to a bulk sample derived from a single primary sample, whereas MRLs for plant products, eggs and dairy products apply to a composite bulk sample derived from 1-10 primary samples. 3. SAMPLING PROCEDURES Notes. (a) The terms used are defined in Annex I and the procedures are shown schematically i
9、n Annexes IIA and IIB. (b) ISO recommendations for sampling of grain1, or other commodities shipped in bulk may be adopted, if required. 3.1 Precautions to be taken Contamination and deterioration of samples must be prevented at all stages, because they may affect the analytical results. Each lot to
10、 be checked for compliance must be sampled separately. 3.2 Collection of primary samples The minimum number of primary samples to be taken from a lot is determined from Table 1, or Table 2 in the case of a suspect lot of meat or poultry. Each primary sample should be taken from a randomly chosen pos
11、ition in the lot, as far as practicable. The primary samples must consist of sufficient material to provide the laboratory sample(s) required from the lot. Note. (a) Sampling devices required for grain1, pulses2 and tea3 are described in ISO recommendations and those required for dairy products4 are
12、 described by the IDF. 3.3 Preparation of the bulk sample 3.3.1 Procedure for meat and poultry (Table 3) Each primary sample is considered to be a separate bulk sample. 3.3.2 Procedure for plant products, eggs or dairy products (Tables 4 and 5) The primary samples should be combined and mixed well,
13、if practicable, to form the bulk sample. 3.3.3 Alternative procedure where mixing to form the bulk sample is inappropriate or impractical Where units may be damaged (and thus residues may be affected) by the processes of mixing or sub-division of the bulk sample, or where large units cannot be mixed
14、 to produce a more uniform residue distribution, the units should be allocated randomly to replicate laboratory samples at the time of taking the primary samples. In this case, the result to be used should be the mean of valid results obtained from the laboratory samples analyzed. 3.4 Preparation of
15、 the laboratory sample Where the bulk sample is larger than is required for a laboratory sample, it should be divided to provide a representative portion. A sampling device, quartering, or other appropriate size reduction process may be used but units of fresh plant products or whole eggs should not
16、 be cut or broken. Where required, replicate laboratory samples should be withdrawn at this stage or they may be prepared as in 3.3.3, above. The minimum sizes required for laboratory samples are given in Tables 3, 4 and 5. 3.5 Sampling record The sampling officer must record the nature and origin o
17、f the lot; the owner, supplier or carrier of it; the date and place of sampling; and any other relevant information. Any departure from the recommended method of sampling must be recorded. A signed copy of the record must accompany each replicate laboratory sample and a copy should be retained by th
18、e sampling officer. A copy of the sampling record should be given to the owner of the lot, or a representative of the owner, whether or not they are to be provided with a laboratory sample. If sampling CAC/GL 33 Page 3 of 20 records are produced in computerised form, these should be distributed to t
19、he same recipients and a similar verifiable audit trail maintained. 3.6 Packaging and transmission of the laboratory sample The laboratory sample must be placed in a clean, inert container which provides secure protection from contamination, damage and leakage. The container should be sealed, secure
20、ly labelled and the sampling record must be attached. Where a bar code is utilised, it is recommended that alphanumeric information is also provided. The sample must be delivered to the laboratory as soon as practicable. Spoilage in transit must be avoided, e.g. fresh samples should be kept cool and
21、 frozen samples must remain frozen. Samples of meat and poultry should be frozen prior to despatch, unless transported to the laboratory before spoilage can occur. 3.7 Preparation of the analytical sample The laboratory sample should be given a unique identifier which, together with the date of rece
22、ipt and the sample size, should be added to the sample record. The part of the commodity to be analysed5,6, i.e. the analytical sample, should be separated as soon as practicable. Where the residue level must be calculated to include parts which are not analysed, the weights of the separated parts m
23、ust be recorded. 3.8 Preparation and storage of the analytical portion The analytical sample should be comminuted, if appropriate, and mixed well, to enable representative analytical portions to be withdrawn. The size of the analytical portion should be determined by the analytical method and the ef
24、ficiency of mixing. The methods for comminution and mixing should be recorded and should not affect the residues present in the analytical sample. Where appropriate, the analytical sample should be processed under special conditions, e.g. at sub-zero temperature, to minimize adverse effects. Where p
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