DIN EN 12393-2-2014 Foods of plant origin - Multiresidue methods for the determination of pesticide residues by GC or LC-MS MS - Part 2 Methods for extraction and cleanup German ve.pdf

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1、March 2014 Translation by DIN-Sprachendienst.English price group 17No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS

2、67.050!%,lEnglish version EN 12393-2:2013,English translation of DIN EN 12393-2:2014-03Pflanzliche Lebensmittel Multiverfahren zur Bestimmung von Pestizidrckstnden mit GC oder LC-MS/MS Teil 2: Verfahren zur Extraktion und Reinigung;Englische Fassung EN 12393-2:2013,Englische bersetzung von DIN EN 12

3、393-2:2014-03Aliments dorigine vgtale Mthodes multirsidus de dtermination de rsidus de pesticides par CPG ouCL-SM/SM Partie 2: Mthodes dextraction et de purification;Version anglaise EN 12393-2:2013,Traduction anglaise de DIN EN 12393-2:2014-03SupersedesDIN EN 12393-2:2014-01www.beuth.deDocument com

4、prises 44 pagesIn case of doubt, the German-language original shall be considered authoritative.02.14DIN EN 12393-2:2014-03 2 A comma is used as the decimal marker. National foreword This document (EN 12393-2:2013) has been prepared by Technical Committee CEN/TC 275 “Food analysis Horizontal methods

5、” (Secretariat: DIN, Germany), Working Group WG 4 “Pesticides in food of plant origin” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Lebensmittel und landwirtschaftliche Produkte (Food and Agricultural Products Standards Committee), Work

6、ing Committee NA 057-01-08 AA Pestizide. Amendments This standard differs from DIN EN 12393-2:2009-01 as follows: a) method L: “Extraction with acetone, liquid-liquid partition with dichloromethane and clean-up on a silicagel/charcoal column” has been deleted; b) methods N and P now also allow the s

7、eparation of analytes by liquid chromatography with MS/MS-detection; c) the scope of method N has been extended to include a definite range of pesticides and their validation data; d) information on GC-MS/MS detection has been incorporated; e) the standard has been editorially revised and references

8、 have been updated. Compared with DIN EN 12393-2:2014-01, the following corrections have been made to the German version only and therefore do not affect the English text: a) Foreword, fourth paragraph, first line: “EN 12393-3:2008” has been corrected to read “EN 12393-2:2008”; b) in Subclause 6.6,

9、fifth paragraph, last sentence (i.e. before the NOTE), “2 ml” has been corrected to “4 ml”: “. Endvolumen von 4 ml .” (. the obtained 4 ml .); c) Subclause 6.8 Table 4: The text “Tabelle 4 (fortgesetzt)” (Table 4 (continued) is to be repeated at the top of each page of the table; d) Subclause 6.9, l

10、ine 1: “4” has been corrected to read “3”: “Die Pestizide, die mit diesem Verfahren bestimmt werden knnen, sind in Tabelle 3 aufgefhrt.” (The pesticides that can be analysed by this method are listed in Table 3.) Previous editions DIN EN 12393-2: 1998-12, 2009-01, 2014-01 EUROPEAN STANDARD NORME EUR

11、OPENNE EUROPISCHE NORM EN 12393-2 November 2013 ICS 67.050 Supersedes EN 12393-2:2008English Version Foods of plant origin - Multiresidue methods for the determination of pesticide residues by GC or LC-MS/MS - Part2: Methods for extraction and clean-up Aliments dorigine vgtale - Mthodes multirsidus

12、de dtermination de rsidus de pesticides par CPG ou CL-SM/SM - Partie 2: Mthodes dextraction et de purificationPflanzliche Lebensmittel - Multiverfahren zur Bestimmung von Pestizidrckstnden mit GC oder LC-MS/MS - Teil 2: Verfahren zur Extraktion und Reinigung This European Standard was approved by CE

13、N on 21 September 2013. CEN members are bound to comply with the CEN/CENELEC Internal Regulations 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 standa

14、rds may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. 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 not

15、ified to the CEN-CENELEC Management Centre has the same status as the official versions. 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, I

16、celand, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, 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 Ma

17、nagement Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 12393-2:2013: EEN 12393-2:2013 (E) 2 Contents Page Foreword 3 Introduction .4 1 Scope 5 2 Normative references 5 3 Principles 5

18、 4 General: Summary of procedures 6 5 Method M: Extraction with acetone and liquid-liquid partition with dichloromethane/light petroleum, if necessary clean-up on Florisil 7 6 Method N: Extraction with acetone, liquid-liquid partition with dichloromethane or cyclohexane/ethyl acetate, clean-up with

19、gel permeation and silica gel chromatography 10 7 Method P: Extraction with ethyl acetate, and if necessary, clean-up by gel permeation chromatography 35 Annex A (informative) Average water content of crops and foods . 41 Bibliography . 42 DIN EN 12393-2:2014-03 EN 12393-2:2013 (E) 3 Foreword This d

20、ocument (EN 12393-2:2013) has been prepared by Technical Committee 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 l

21、atest by May 2014, and conflicting national standards shall 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 p

22、atent rights. This document supersedes EN 12393-2:2008. In comparison with EN 12393-2:2008, the following significant technical changes have been made: a) implementation of liquid chromatography in combination with tandem mass spectrometry (LC-MS/MS) for the quantification and/or confirmation of pes

23、ticide residues; b) incorporation of information on GC-MS/MS; c) deletion of method L as no longer in use; d) editorial updating of the document according to references, etc; e) enlargement of scope of method N concerning number of pesticides and validation data. EN 12393, Foods of plant origin Mult

24、iresidue 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 each of the analytical selected methods; Part 2 “Metho

25、ds 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 confirmatory tests“ gives some recommended technique

26、s 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 European Standard: Austria, Belgium, Bulgaria, Croat

27、ia, 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, Slovenia, Spain, Sweden, Switzerland, Turkey and th

28、e United Kingdom. DIN EN 12393-2:2014-03 EN 12393-2:2013 (E) 4 Introduction This European 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 incl

29、uded in this European Standard have been validated and/or are widely used throughout 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, extra

30、ction, clean-up and chromatographic conditions are appropriate to improve method performance, see Clause 3. DIN EN 12393-2:2014-03 EN 12393-2:2013 (E) 5 1 Scope This European Standard specifies methods for the extraction and clean-up of food samples of plant origin for quantitative determination of

31、pesticide residues. Different solvents can be used for this purpose. These pesticide residues are generally associated with other co-extracted compounds which would interfere in the analysis. To purify the crude extracts to be analysed, several techniques can be used. This European Standard contains

32、 the following extraction and clean-up 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 N: Extracti

33、on 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 by gel permeation chromatography 6. This European Standard specifies the

34、 details of methods M, N and P for the extraction and the clean-up of food samples of plant origin. Several solvents at different volumes are used for extraction. Techniques of clean-up are listed such as liquid-liquid partition, liquid chromatography on various adsorbents and gel permeation chromat

35、ography. A table providing the couples (matrix/pesticide) which have been submitted to collaborative studies and a list of indicative applicability of the method to different pesticides are given for each method, wherever possible. 2 Normative references The following documents, in whole or in part,

36、 are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 12393-1:2013, Foods of plant origin Multiresidue

37、methods for the determination of pesticide residues by GC or LC-MS/MS Part 1: General considerations 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 Principles As already describe

38、d in the introduction, in certain occasions it is possible to improve the method performance by variations in equipment used, extraction, clean-up and chromatographic conditions. Such variations shall be always clearly documented and demonstrated to give valid results. The pesticide residues are ext

39、racted from the sample by the use of appropriate solvents, so as to obtain the maximum efficiency of extraction of the pesticide residues and minimum co-extracted substances which can give rise to interferences in the determination. Any interfering materials are removed from the sample extract to ob

40、tain a solution of the extracted pesticide residues in a solvent which is suitable for quantitative examination by the selected method of determination. 1) Florisil,is an example of a suitable product available commercially from U.S. Silica company. This information is given for convenience of users

41、 of this standard and does not constitute an endorsement by CEN of this product. DIN EN 12393-2:2014-03 EN 12393-2:2013 (E) 6 4 General: Summary of procedures 4.1 Extraction The extraction procedures are summarized in Table 1. Table 1 Extraction procedures Methods Mass of samples (MS) Volume of solv

42、ent (VS) Ratio (MS/ VS) g ml g/ml M 100 Acetone: 200 N 100 aAcetone: 200 P 10 Ethyl acetate: 20 aOnly relevant if the water content of the matrix is greater than 70 %. 4.2 Clean-up 4.2.1 Liquid-liquid partition The liquid-liquid partition procedures are summarized in Table 2. Table 2 Liquid-liquid p

43、artition Method Aliquot portion of extract Volume of added water Volume of solvent Ratio (AE) ml (VW) ml (VS) ml AE/ VWM 80 0 200 - aN 200 x a100 - aaDepends on the water content of the matrix. Two techniques of liquid-liquid partition are proposed: with added water (method N); no added water (metho

44、d M). 4.2.2 Adsorption column chromatography Methods: M, N with different adsorbents: silica gel, charcoal, Florisil, used pure or in mixture. 4.2.3 Gel permeation chromatography with Bio-Beads S-X32)Method N, and, if needed, method P. 2) BioBeads S-X3 is an example of a suitable product available c

45、ommercially. This information is given for convenience of users of this standard and does not constitute an endorsement by CEN of this product. DIN EN 12393-2:2014-03 EN 12393-2:2013 (E) 7 5 Method M: Extraction with acetone and liquid-liquid partition with dichloromethane/light petroleum, if necess

46、ary clean-up on Florisil 5.1 Principle The chopped test portion is homogenized in acetone and the homogenate is filtered. An aliquot portion of the filtrate is extracted with a mixture of light petroleum and dichloromethane and then with dichloromethane. The organic phase can be injected directly wi

47、thout clean-up into a gas chromatograph with an appropriate detector or purified on a Florisil column. Either mixtures of diethyl ether and light petroleum (method M1) or mixtures of dichlormethane, light petroleum and acetonitrile (method M2) are used for the elution of analytes from Florisil. The

48、eluates are concentrated for examination by GC. 5.2 Reagents 5.2.1 General All reagents shall be suitable for the analysis of pesticide residues and in accordance with EN 12393-1:2013, Clause 4. 5.2.2 Acetone 5.2.3 Light petroleum, boiling range 40 C to 60 C 5.2.4 Sodium chloride Heat at 500 C for a

49、t least 4 h, allow to cool, and store in a stoppered bottle. 5.2.5 Dichloromethane 5.2.6 Acetonitrile 5.2.7 Sodium sulfate Heat at 500 C for at least 4 h, allow to cool, and store in a stoppered bottle. 5.2.8 Florisil (or equivalent), 150 m to 250 m (60 mesh to 100 mesh) Activate by heating at 130 C to 135 C for at least 5 h, allow to cool in a desiccator and transfer to an airtight stoppered jar. The adsorbent thus treated keeps its activity only for four days. It can subsequently b