METHOD VALIDATION AND QUALITY CONTROL PROCEDURES
FOR
PESTICIDE RESIDUES ANALYSIS IN FOOD AND FEED
Document N° SANCO/2007/3131
31/October/2007
Superdes Document No. SANCO/10232/2006
Table of contents Introduction (3)
Accreditation (3)
Sampling, transport, processing and storage of samples (3)
Sampling (3)
Laboratory sample transportation (4)
Sample preparation and processing prior to analysis (4)
Pesticide standards, calibration solutions, etc (5)
Identity, purity, and storage of standards (5)
Preparation and storage of stock standards (5)
Preparation, u and storage of working standards (6)
Testing and replacement of standards (6)
Extraction and concentration (6)
辣炒扇贝Extraction conditions and efficiency (6)
Extract concentration and dilution to volume (7)
Contamination and interference (7)
Contamination (7)
Interference (8)
Analytical calibration, reprentative analytes, matrix effects and chromatographic integration (8)
General requirements (8)
Calibration (8)
Reprentative analytes (9)
Matrix effects and matrix-matched calibration (10)
Standard addition (11)
Effects of pesticide mixtures on calibration (11)
Calibration for pesticides that are mixtures of isomers, etc (11)电子邮箱注册申请
Calibration using derivatives or degradation products (12)
Chromatographic integration (12)
Analytical method validation and performance criteria (12)
Method validation (12)
Methods for determination of fat or dry weight content (13)
Routine recovery determination (13)
Acceptability of analytical performance for routine recoveries (14)
Proficiency testing and analysis of reference materials (15)
Confirmation of results (15)
Principles of confirmation (15)
Chromatographic paration (16)
Confirmation by mass spectrometry (MS) (16)
Confirmation by an independent laboratory (18)
Reporting of results (18)
Expression of results (18)
Calculation of results (19)
Qualifying results with uncertainty data (19)
Interpretation of results (20)
Annex 1 (22)
Selection of reprentative matrices (22)
Appendix 1 (24)
Glossary (24)
METHOD VALIDATION AND QUALITY CONTROL PROCEDURES
FOR
PESTICIDE RESIDUES ANALYSIS IN FOOD AND FEED
Introduction
盐城旅游鸭嘴鱼怎么做好吃1.The guidance in this document is intended for the monitoring of pesticide residues in the European Union. The document describes the method validation and analytical quality control (AQC) requirements to support the validity of data ud for checking compliance with maximum residue limits (MRLs), enforcement actions, or asssment of consumer exposure to pesticides1.
The key objectives are:
(i)to provide a harmonized cost-effective quality
assurance system in the EU
(ii)to ensure the quality and comparability of analytical
野兽英语results
(iii)to ensure that acceptable accuracy is achieved
(iv)to ensure that fal positives or fal negatives are
not reported
董生与李氏(v)to support compliance with ISO/IEC 17025
(accreditation standard)
2.This document is complementary and integral to the requirements in ISO/IEC 17025.
3.This document superdes Document No. SANCO/10232/2006.
4.The glossary (Appendix 1) should be consulted for explanation of terms ud in the text.
Accreditation
5.In accordance with Article 12 of Regulation 882/2004, laboratories designated for official control of pesticide residues must be accredited to ISO/IEC 17025, or avail of the derogation in Article 18 of Regulation 2076/2005. The quality control system of tho laboratories availing of Article 18 should be bad on the requirements described in this document, which is intended as guidance for accreditation purpos.
Sampling, transport, processing and storage of samples
Sampling
6.Laboratory samples should be taken in accordance with Directive 2002/63/EC or superding legislation. Where it is impractical to take primary samples randomly within a lot, the method of sampling must be recorded.
1 For samples of animal origin the guidance in this document shall enter into force 6 month from the publication of the last of the Annexes I, II, III and IV of Regulation no 396/2005.
Laboratory sample transportation
7.Samples must be transported to the laboratory in clean containers and robust packaging. Polythene bags, ventilated if appropriate, are acceptable for most samples but low-permeability bags (e.g. nylon film) must be ud for samples to be analyd for residues of fumigants. Samples of commodities pre-packed for retail sale should not be removed from their packaging before trans-port. Very fragile or perishable products (e.g. ripe raspberries) may have to be frozen to avoid spoilage and then transported in “dry ice” or similar, to avoid thawing in transit. Samples that are froz
en at the time of collection must be transported without thawing. Samples that may be damaged by chilling (e.g. bananas) must be protected from both high and low temperatures.
8.Rapid transportation to the laboratory, preferably within one day, is esntial for samples of most fresh products. The condition of samples delivered to the laboratory should approximate to that acceptable to a discerning purchar, otherwi samples should normally be considered unfit for analysis.
9.Samples must be identified clearly and indelibly, in a way that prevents inadvertent loss or confusion of labelling. The u of marker pens containing organic solvents should be avoided for labelling bags containing samples to be analyd for fumigant residues, especially if an electron capture detector is to be ud.
Sample preparation and processing prior to analysis
10.On receipt, each laboratory sample must be allocated a unique reference code by the laboratory.
11.Sample preparation, sample processing and sub-sampling to obtain analytical portions should take place before visible deterioration occurs. This is particularly important when the analytical result
is to be ud to asss consumer intake. Canned, dried or similarly procesd samples should be analyd within the stated shelf life.
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12.Sample preparation must be in accordance with the definition of the commodity and the part(s) to be analyd, e Regulation 396/2005 Annex1.
13.Sample processing and storage procedures should be demonstrated to have no significant effect on the residues prent in the analytical sample (e Directive 2002/63/EC). Where there is evidence that comminution (cutting and homogenisation) at ambient temperature has a significant influence on the degradation of certain pesticide residues, it is recommended that samples are homogenid at low temperature (e.g. frozen and/or in the prence of “dry ice”). Otherwi, application of a higher measurement uncertainty with the reported results should be considered for tho pesticides. Where comminution is known to affect residues (e.g. dithiocarbamates or fumigants) and practical alternative procedures are not available, the test portion should consist of whole units of the commodity, or gments removed from large units. For all other analys, the whole laboratory sample (in most cas 1-2 kg) needs to be communited. All analys should be undertaken within the shortest time practicable, to minimi sample storage. Analys for residues of very labile or volatile pesticides should be started, and the procedures involved in potential loss of an
alyte completed, on the day of sample receipt. In any ca, sample comminution should ensure that the sample is homogeneous enough so that sub-
sampling variability is acceptable. If this is not achievable, the u of larger test portions should be considered.
14.If a single analytical portion is unlikely to be reprentative of the analytical sample, replicate portions must be analyd, to provide a better estimate of the true value.
Pesticide standards, calibration solutions, etc.
Identity, purity, and storage of standards
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15.“Pure” standards of analytes and internal standards should be of known purity and each must be uniquely identified and the date of receipt recorded. They should be stored at low temperature, preferably in a freezer, with light and moisture excluded, i.e. under conditions that minimi the rate of degradation. Under such conditions, the supplier’s expiry date, which is often bad on less stringent storage conditions, may be replaced, as appropriate for each standard, by a date allowing for storage up to 10 years. The pure standard may be retained if its purity is shown to remain accept
able. The purity should be checked by the allocated time after which a “pure” standard may be retained if its purity is shown to remain acceptable and a new expiry date is allocated. Ideally, the identity of freshly acquired “pure” standards should be checked if the analytes are new to the laboratory.
Preparation and storage of stock standards
16.When preparing stock standards (solutions, dispersions or gaous dilutions) of “pure” standards of analytes and internal standards, the identity and mass (or volume, for highly volatile compounds) of the “pure” standard and the identity and amount of the solvent (or other diluents) must be recorded. The solvent(s) must be appropriate to the analyte (solubility, no reaction) and method of analysis. Moisture must be excluded during equilibration of the “pure” standard to room temperature before u and concentrations must be corrected for the purity of the “pure” standard.
17.Not less than 10 mg of the “pure” standard should be weighed using a 5 decimal place balance. The ambient temperature should be that at which the glassware is calibrated, otherwi preparation of the standard should be bad on mass measurement. Volatile liquid analytes should be dispend by weight or volume (if the density is known) directly into solvent. Gaous (fumigant) ana
lytes may be dispend by bubbling into solvent and weighing the mass transferred, or by preparing gaous dilutions (e.g. with a gas-tight syringe, avoiding contact with reactive metals).
18.Stock standards must be labelled indelibly, allocated an expiry date and stored at low temperature in the dark in containers that prevent any loss of solvent and entry of water. Currently available data show that stock standards of the large majority of pesticides in toluene and acetone are stable for at least 5 years in the freezer when stored in tightly clod glass containers.
19.When a stock standard is prepared for the first time, and for suspensions (e.g. dithiocarbamates) and solutions (or gaous dilutions) of highly volatile fumigants that must be prepared freshly, the accuracy of the solution should be compared with a cond solution made independently at the same time.
