1、BSI Standards PublicationBS EN 12393-1:2013Foods of plant origin Multiresidue methods for thedetermination of pesticideresidues by GC or LC-MS/MSPart 1: General considerationsCopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or netwo
2、rking permitted without license from IHS-,-,-BS EN 12393-1:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 12393-1:2013. It supersedes BS EN 12393-1:2008 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee AW/275,
3、 Food analysis - Horizontal methods.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Inst
4、itution 2013. Published by BSI Standards Limited 2013ISBN 978 0 580 77445 4 ICS 67.050; 67.080.01 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 November 201
5、3.Amendments issued since publicationDate T e x t a f f e c t e dCopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 12393-1:2013EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NO
6、RM EN 12393-1 November 2013 ICS 67.050 Supersedes EN 12393-1:2008English Version Foods of plant origin - Multiresidue methods for the determination of pesticide residues by GC or LC-MS/MS - Part 1: General considerations Aliments dorigine vgtale - Mthodes multirsidus de dtermination de rsidus de pes
7、ticides par CPG ou CL-SM/SM - Partie 1: Gnralits Pflanzliche Lebensmittel - Multiverfahren zur Bestimmung von Pestizidrckstnden mit GC oder LC-MS/MS - Teil 1: Allgemeines This European Standard was approved by CEN on 21 September 2013. CEN members are bound to comply with the CEN/CENELEC Internal Re
8、gulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN me
9、mber. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions.
10、 CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Polan
11、d, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation i
12、n any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 12393-1:2013: ECopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 12393-1:2013EN 12393-1:2
13、013 (E) 2 Contents Page Foreword 3 Introduction .4 1 Scope 5 2 Normative references 5 3 Principle 5 4 Reagents .6 5 Apparatus .9 6 Procedure 11 7 Determination 13 8 Confirmatory tests 14 9 Evaluation of results 14 10 Test report . 15 Annex A (informative) Purification of solvents and reagents 16 Bib
14、liography . 17 Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 12393-1:2013EN 12393-1:2013 (E) 3 Foreword This document (EN 12393-1:2013) has been prepared by Technical Com
15、mittee CEN/TC 275 “Food analysis - Horizontal methods”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by May 2014, and conflicting national standards shall
16、be withdrawn at the latest by May 2014. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 12393-1:2008. The
17、following significant technical changes have been made: a) separation of analytes by liquid chromatography with MS/MS-detection in methods N and P; b) incorporation of information on GC-MS/MS detection; c) deletion of method L as no longer in use; d) editorial updating of the document according to r
18、eferences, etc. EN 12393, Foods of plant origin Multiresidue methods for the determination of pesticide residues by GC or LC-MS/MS is divided into three parts: Part 1 “General considerations“ provides general considerations with regard to reagents, apparatus, gas chromatography, etc., applying to ea
19、ch of the selected analytical methods; Part 2 “Methods for extraction and clean-up“ presents methods M, N and P for the extraction and clean-up using techniques such as liquid-liquid partition, adsorption column chromatography or gel permeation column chromatography, etc.; Part 3 “Determination and
20、confirmatory tests“ gives some recommended techniques for the qualitative and the quantitative measurements of residues and the confirmation of the results. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this
21、European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia,
22、 Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 12393-1:2013EN 12393-1:2013 (E) 4 Introduction This Eu
23、ropean Standard comprises a range of multi-residue methods of equal status: no single method can be identified as the prime method because, in this field, methods are continuously developing. The selected methods included in this European Standard have been validated and/or are widely used throughou
24、t Europe. Because these methods can be applied to the very wide range of food commodities/pesticide combinations, using different systems for determination, there are occasions when variations in equipment used, extraction, clean-up and chromatographic conditions are appropriate to improve method pe
25、rformance, see 3.1. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 12393-1:2013EN 12393-1:2013 (E) 5 1 Scope This European Standard gives general considerations for the de
26、termination of pesticide residues in foods of plant origin. Each method specified in this European Standard is suitable for identifying and quantifying a definite range of those organohalogen, and/or organophosphorus and/or organonitrogen pesticides which occur as residues in foodstuffs of plant ori
27、gin. This European Standard contains the following methods that have been subjected to interlaboratory studies and/or are adopted throughout Europe: method M: Extraction with acetone and liquid-liquid partition with dichloromethane/light petroleum, if necessary clean-up on Florisil 1)1, 2, 3; method
28、 N: Extraction with acetone, liquid-liquid partition with dichloromethane or cyclohexane/ethyl acetate and clean-up with gel permeation and silica gel chromatography 4, 5; method P: Extraction with ethyl acetate and, if necessary, clean-up with gel permeation chromatography 6. The applicability of t
29、he three methods M, N and P for residue analysis of organohalogen, organophosphorus and organonitrogen pesticides, respectively, is given for each method. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its ap
30、plication. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 12393-2:2013, Foods of plant origin Multiresidue methods for the determination of pesticide residues by GC or LC-MS/MS Part 2:
31、 Methods for extraction and clean-up EN 12393-3:2013, Foods of plant origin Multiresidue methods for the determination of pesticide residues by GC or LC-MS/MS Part 3: Determination and confirmatory tests 3 Principle 3.1 General As already described in the introduction, in certain occasions it is pos
32、sible to improve the method performance by variations in equipment used, extraction, clean-up and chromatographic conditions. Such variations shall always be clearly documented and demonstrated to give valid results. The methods described in this European Standard are based on a four-stage process (
33、in some cases two stages may be combined, in whole or in part), as given in 3.2 to 3.5. 1) Florisil is an example of a suitable product available commercially. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of this produ
34、ct. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 12393-1:2013EN 12393-1:2013 (E) 6 Quality control procedures for pesticide residue analysis, e.g. published by the Europ
35、ean Commission 7, should be followed in its updated versions. The principles laid down in this guidance document such as initial method validation, on-going performance verification and calibration should be followed carefully in order to ensure a proper use of different combinations of separation a
36、nd detection methods. Also, further information such as in 8 might be helpful. 3.2 Extraction Extraction of the residues from the sample matrix by the use of appropriate solvents, so as to obtain the maximum efficiency of extraction of the residues and minimum co-extraction of any substances which c
37、an give rise to interferences in the determination. 3.3 Clean-up Removal of interfering materials from the sample extract to obtain a solution of the extracted residue in a solvent which is suitable for determination by the selected method of determination. 3.4 Determination Gas chromatography (GC)
38、with selective detectors may be used: electron-capture detection (ECD) for organohalogen, thermionic detector (NPD, P-mode or N/P mode) for organophosphorus and organonitrogen compounds and flame-photometric detector (FPD) for organophosphorus and organosulfurous pesticides. Hall detector (ECHD), at
39、omic emission detector (AED) and mass spectrometry (MS) and tandem mass spectrometry may also be used for a large class of pesticides. As alternative, liquid chromatography (LC) with MS-MS-detection has been proven to be successful. 3.5 Confirmation Procedures to confirm the identity and quantity of
40、 observed residues should be used, particularly in those cases where it would appear that the maximum residue limit (MRL) has been exceeded. 3.6 Use of internal standards An internal standard may be added in a constant amount to samples, the blank and calibration standards. This substance can be use
41、d for checking critical points of methods (e.g. volatile or unstable compounds) and/or for quantification purposes, if appropriate. This is done to correct for the loss of analyte during sample preparation and sample clean-up or to check reproducibility of final determination steps by GC or LC. The
42、internal standard should be preferably a compound that has very similar physico-chemical and chemical properties compared to the analyte. 4 Reagents 4.1 General Use reagents of purity suitable for pesticide residue analysis and check their purity (see 4.2). If required, purify water and solvents use
43、d, e.g. as described in Annex A, and check their purity (see 4.2). Purify and periodically activate adsorbents according to the requirements of the different analytical methods; check their purity (see 4.2). Take every precaution to avoid possible contamination of water, solvents, adsorbents, etc. f
44、rom plastics and rubber materials. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 12393-1:2013EN 12393-1:2013 (E) 7 4.2 Check for purity of reagents 4.2.1 Solvents Concent
45、rate solvents by the factor involved in the respective method to be used. Test for purity under the same conditions as used in the method. The chromatogram should not show any interfering impurity. 4.2.2 Water Extract 10 parts by volume of water with one part by volume of n-hexane or light petroleum
46、, dichloromethane or any other non-water miscible solvent used in the method. Separate the organic phase, concentrate by the factor involved in the respective method and test for purity under the same conditions as used in the method. The chromatogram should not show any interfering impurity. 4.2.3
47、Inorganic salts Extract inorganic salts, for example sodium chloride, after purification according to Annex A or the requirements of the different analytical methods. Extract the salts and any aqueous solution used, with n-hexane or light petroleum, dichloromethane or any other non-water miscible so
48、lvent used in the method. Concentrate the extract by the factor involved in the respective method and test the purity under the same conditions as used in the method. The chromatogram should not show any interfering impurity. 4.2.4 Adsorbents Elute an amount of adsorbent equal to that used in the an
49、alytical method with the corresponding type and volume of solvent or solvent mixture. Concentrate the eluate as indicated in the analytical method and test for purity. The chromatogram should not show any interfering impurity. Check the activity of adsorbents regularly as described in the methods M to P
