EN 15662-2018 Foods of plant origin - Multimethod for the determination of pesticide residues using GC- and LC-based analysis following acetonitrile extraction .pdf

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1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Foods of plant origin - Multimethod for the determination of pesticide residues using GC- and LC-based analysis following acetonitrile extraction/partitioning and clean-up by dispersive SPE - Modular QuEChERS-methodBS E

2、N 15662:2018EUROPEANSTANDARDNORME EUROPENNE EUROPISCHE NORMEN 15662 May 2018ICS 67.050 Supersedes EN 15662:2008EnglishVersionFoods of plant origin - Multimethod for the determinationof pesticide residues using GC- and LC-based analysis following acetonitrile extraction/partitioning and clean-up by d

3、ispersive SPE - Modular QuEChERS-method Aliments dorigine vgtale - Multimthode de dtermination desrsidusde pesticides paranalyse CGet CL aprs extraction/partition avec de lactonitrileet purification par SPEdispersive - Mthode modulaire QuEChERSPflanzliche Lebensmittel - Multiverfahren zurBestimmung

4、von Pestizidrckstnden mit GC und LCnach Acetonitril-Extraktion/Verteilung und Reinigung mit dispersiver SPE - Modulares QuEChERS-VerfahrenThis European Standard was approved by CEN on 27 December2017.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the condit

5、ions for giving thisEuropean Standard the status of a national standard without any alteration.Up-to-date lists and bibliographical referencesconcerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in

6、three official versions (English, French, German). A version in any other language made bytranslation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC ManagementCentre has the same status as the officialversions.CEN members are the nationalstandards bodi

7、es 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, Poland, Portugal, Romania, Serbia, Slovakia, Slov

8、enia, Spain, Sweden, Switzerland, Turkey and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGCEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels 2018 CEN All rights of exploitation in any form and by any means reserved

9、worldwide for CENnational Members.Ref. No. EN 15662:2018 ENational forewordThis British Standard is the UK implementation of EN 15662:2018. It supersedes BS EN 15662:2008, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee AW/275, Food analysis - Horizont

10、al 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 Institution 2018 Published by

11、 BSI Standards Limited 2018ISBN 978 0 580 94294 5ICS 67.050Compliance 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 June 2018.Amendments/corrigenda issued since publi

12、cationDate Text affectedBRITISH STANDARDBS EN 15662:2018EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15662 May 2018 ICS 67.050 Supersedes EN 15662:2008English Version Foods of plant origin - Multimethod for the determination of pesticide residues using GC- and LC-based analysis following ace

13、tonitrile extraction/partitioning and clean-up by dispersive SPE - Modular QuEChERS-method Aliments dorigine vgtale - Multimthode de dtermination des rsidus de pesticides par analyse CG et CL aprs extraction/partition avec de lactonitrile et purification par SPE dispersive - Mthode modulaire QuEChER

14、S Pflanzliche Lebensmittel - Multiverfahren zur Bestimmung von Pestizidrckstnden mit GC und LC nach Acetonitril-Extraktion/Verteilung und Reinigung mit dispersiver SPE - Modulares QuEChERS-VerfahrenThis European Standard was approved by CEN on 27 December 2017. CEN members are bound to comply with t

15、he 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 standards may be obtained on application to the CEN-CENELEC Manageme

16、nt 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 notified to the CEN-CENELEC Management Centre has the same status

17、 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, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,

18、Netherlands, Norway, Poland, Portugal, Romania, Serbia, 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: Rue de la Science 23, B-1040 Brussels

19、 2018 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15662:2018 EBS EN 15662:2018EN 15662:2018 (E) 2 Contents Page European foreword . 3 1 Scope 4 2 Normative references 4 3 Principle . 4 4 Preparation and storage of the samples .

20、 4 5 Procedure. 5 6 Evaluation of results . 15 7 Confirmatory tests . 22 8 Precision 22 9 Test report 22 Annex A (informative) Description of modules 23 Annex B (informative) Complementary information . 76 Annex C (informative) Abbreviations 78 Bibliography . 80 BS EN 15662:2018EN 15662:2018 (E) 3 E

21、uropean foreword This document (EN 15662:2018) 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

22、endorsement, at the latest by November 2018, and conflicting national standards shall be withdrawn at the latest by November 2018. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying a

23、ny or all such patent rights. This document supersedes EN 15662:2008. With the revised version, some amendments and improvements have been taken into consideration, notably: the more precise differentiation between feasible modes of operation (Table 1 to Table 5); the opportunity to report the appli

24、ed modes of operation (e.g. extraction or clean-up modules) in a simple way; clear indications of approved modes of operation for particular commodities (Table 6); the optimization of extraction efficiency by longer extraction time; the specification of suitable parameters for the detection with UPL

25、C-MS/MS and GC-MS/MS; new approaches for the quantitation of pesticide residues including a simplified procedure for the calculation of residue levels; references to the improved validation data for the method (see Table 7 and CEN/TR 17063); a list of abbreviations has been added in Annex C. WARNING

26、 The application of this standard may involve hazardous materials, operations and equipment. This standard does not claim to address all the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and to dete

27、rmine the applicability of regulatory limitations prior to use. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Esto

28、nia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 15662:201

29、8EN 15662:2018 (E) 4 1 Scope This European Standard stipulates a method for the analysis of pesticide residues in foods of plant origin, such as fruits (including dried fruits), vegetables (including dried vegetables), cereals and many processed products thereof by using GC, GC-MS(/MS), and/or LC-MS

30、(/MS). The method has been collaboratively studied on a large number of commodity/pesticide combinations. Precision data are summarized in CEN/TR 17063. Guidelines for calibration are outlined in CEN/TS 17061. 2 Normative references The following documents are referred to in the text in such a way t

31、hat some or all of their content constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. CEN/TS 17061:2017, Foodstuffs - Guidelines for the calibration a

32、nd quantitative determination of pesticide residues and organic contaminants using chromatographic methods 3 Principle The homogeneous sample is extracted with the help of acetonitrile. Samples with low water content ( 40 % and 40 % to 80 %) and high matrix load or high oil content (5 %) Garlic, avo

33、cados E7 A test portion of 2 g is completed with 10 ml of water and then extracted with acetonitrile Plant material and edibles with very low water content ( 70 %, inacceptable losses of fat soluble pesticides did not occur. gIf the recovery of anthracen is 70 %, inacceptable losses planar pesticide

34、s during clean-up with graphitized carbon black did not occur. + very good detectable + good detectable + poor detectable not applicable BS EN 15662:2018EN 15662:2018 (E) 26 A.2 Apparatus used in all extraction (E) and clean-up (C) and stabilization (S) modules Usual laboratory apparatus and, in par

35、ticular, the following: A.2.1 Centrifuge tubes with screw caps, 50 ml: For example: a) 50 ml centrifuge tubes made of poly-tetrafluoroethylene with screw caps, or b) disposable 50 ml polypropylene centrifuge tubes with screw caps. A.2.2 10 ml solvent-dispenser for acetonitrile; to be employed for do

36、sing of extraction solvent. A.2.3 Automatic pipettes, suitable for handling volumes of 10 l to 100 l, 200 l to 1 000 l and 1 ml to 10 ml, or 10 ml graduated glass pipettes. A.2.4 Polypropylene-single use centrifuge tubes with screw caps, 10 ml or 12 ml. A.2.5 Shaker, horizontal, vertical or orbital

37、shaker, at least 200 min1.A.2.6 Centrifuges, suitable for the centrifuge tubes employed in the procedure (A.2.1, A.2.4) and capable of achieving at least 3000 g. A.2.7 High speed dispersing device, the diameter of the dispersing elements should fit the openings of the centrifuge tubes (A.2.1) used.

38、A.2.8 Grinding device A.2.9 Heated shaker, e.g. shaking waterbath or AGYTAX SR1 CP571)A.2.10 Freezer, operating at 18 C to 25 C. A.2.11 Injection vials, 1,5 ml, suitable for GC and LC autosampler, if necessary with micro-inserts. A.2.12 Screw capped glass vials, 10 ml or 20 ml, for the storage of ex

39、cessive amounts of the final extract, if necessary. A.2.13 Vortex mixer. A.3 Description of extraction (E) modules A.3.1 Module E1: Extraction of a 10 g test portion without additional water using acetonitrile A.3.1.1 Principle This extraction module is used for plant material and food containing 80

40、 % water, like fruits and vegetables and juices. Table 6 shows the commodities extracted preferably with this extraction module. 1) AGYTAXis a product supplied by Cirtalab (Spain). This information is given for the convenience of users of this European Standard and do not constitute an endorsement b

41、y CEN of the products named. Equivalent products may be used if they can be shown to lead to the same results. BS EN 15662:2018EN 15662:2018 (E) 27 The homogeneous sample is extracted in frozen condition (if possible) with acetonitrile. After addition of magnesium sulfate, sodium chloride and buffer

42、ing citrate salts (pH 5 to pH 5,5), the mixture is shaken intensively and centrifuged for phase separation. An aliquot of the organic phase is separated and cleaned-up according to clean-up modules (modules C) if necessary. A.3.1.2 Procedure A.3.1.2.1 Test portion Transfer a representative test port

43、ion of 10 g 0,1 g (samplem ) of the comminuted homogenous sample into a 50 ml centrifuge tube (A.2.1). A.3.1.2.2 Optional ISTD addition Add a defined small volume of the ISTD solution (A.1.2) (addISTDV , e. g. 100 l) containing one or several of the compounds listed in Table A1 at the concentrations

44、 exemplary given (CISTD) A.3.1.2.3 First extraction Add 10 ml of acetonitrile (A.1.3) (VEx). Close the tube and shake samples having room temperature vigorously for 1 min to 3 min or frozen samples for 15 min, using a shaker (A.2.5) if necessary. Samples should be extracted frozen or while in the pr

45、ocess of thawing. If samples are employed for extraction at ambient temperature, it shall be ensured that no significant degradation of the target pesticides occurs. Extended extraction time may be used if shown that it does not affect significantly the recovery rate. If the samples degree of commin

46、ution is insufficient, the extraction can be assisted by a high-speed disperser (A.2.7). In this case the addition of an ISTD prior to the dispersing step is mandatory. The dispersing element is immersed into the sample/acetonitrile mixture and comminution is performed for about 2 min at high speed.

47、 The dispersing element has to be cleaned thoroughly before being used for the next sample to avoid cross-contamination. A.3.1.2.4 Second extraction step and partitioning Add the prepared buffer-salt mixture (A.1.8) to the suspension from A.3.1.2.3. Close the tube and immediately shake vigorously fo

48、r 1 min by hand or 3 min using a shaker (A.2.5) and centrifuge for 5 min at 3000 g. Without delay separate upper acetonitrile layer and pass the obtained raw extract to the clean-up modules C. In the presence of water, magnesium sulfate tends to form lumps, which can harden rapidly. This can be avoi

49、ded, if immediately after the addition of the salt mixture the centrifuge tube is shaken vigorously for few seconds. The 1 min or 3 min extraction of the entire batch may be performed in parallel after the salts were added to all the samples. A.3.1.3 Calculation The mass concentration of the sample in the raw extract raw extractsample gives the ratio of the amount of the sample, from which the residues are extracted, and the extraction volume. Usually raw extractsample is given in g/ml and is calculated by Form