1、Foods of plant origin Multimethod for the determination of pesticideresidues using GC- or LC-basedanalysis following acetonitrileextraction/partitioning andcleanup by dispersive SPE Validation data of the modularQuEChERS-methodPD CEN/TR 17063:2017BSI Standards PublicationNational forewordThis Publis
2、hed Document is the UK implementation of CEN/TR 17063:2017.The UK participation in its preparation was entrusted to TechnicalCommittee AW/275, Food analysis - Horizontal methods.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not
3、 purport to include all the necessary provisions ofa contract. Users are responsible for its correct application. The British Standards Institution 2017.Published by BSI Standards Limited 2017ISBN 978 0 580 94296 9ICS 67.050Compliance with a British Standard cannot confer immunity fromlegal obligati
4、ons.This Published Document was published under the authority of theStandards Policy and Strategy Committee on 30 April 2017.Amendments/corrigenda issued since publicationDate Text affectedPUBLISHED DOCUMENTPD CEN/TR 17063:2017g3g3g3g23g8g6g11g17g12g6g4g15g3g21g8g19g18g21g23g3g21g4g19g19g18g21g23g3g
5、23g8g6g11g17g12g20g24g8g3g23g8g6g11g17g12g22g6g11g8g21g3g5g8g21g12g6g11g23g3CEN/TR 17063 g3 g3g3 g16g131g148g133g138g3g884g882g883g889g3g12g6g22g3g888g889g484g882g887g882g3g8g144g137g142g139g149g138g3g25g135g148g149g139g145g144g3g3g9g145g145g134g149g3g145g136g3g146g142g131g144g150g3g145g148g139g137g
6、139g144g3g486g3g16g151g142g150g139g143g135g150g138g145g134g3g136g145g148g3g150g138g135g3g134g135g150g135g148g143g139g144g131g150g139g145g144g3g145g136g3g146g135g149g150g139g133g139g134g135g3g148g135g149g139g134g151g135g149g3g151g149g139g144g137g3g10g6g486g3g145g148g3g15g6g486g132g131g149g135g134g3g1
7、31g144g131g142g155g149g139g149g3g136g145g142g142g145g153g139g144g137g3g131g133g135g150g145g144g139g150g148g139g142g135g3g135g154g150g148g131g133g150g139g145g144g512g146g131g148g150g139g150g139g145g144g139g144g137g3g131g144g134g3g133g142g135g131g144g151g146g3g132g155g3g134g139g149g146g135g148g149g139
8、g152g135g3g22g19g8g3g486g3g25g131g142g139g134g131g150g139g145g144g3g134g131g150g131g3g145g136g3g150g138g135g3g143g145g134g151g142g131g148g3g20g151g8g6g138g8g21g22g486g143g135g150g138g145g134g3g4g142g139g143g135g144g150g149g3g134g821g145g148g139g137g139g144g135g3g152g177g137g177g150g131g142g135g3g486
9、g3g16g177g150g138g145g134g135g149g3g143g151g142g150g139g146g142g135g149g3g134g135g3g134g177g150g135g148g143g139g144g131g150g139g145g144g3g134g135g149g3g148g177g149g139g134g151g149g3g134g135g3g146g135g149g150g139g133g139g134g135g149g3g146g131g148g3g131g144g131g142g155g149g135g3g6g10g3g145g151g3g6g15g
10、3g131g146g148g176g149g3g135g154g150g148g131g133g150g139g145g144g512g146g131g148g150g139g150g139g145g144g3g131g152g135g133g3g134g135g3g142g821g131g133g177g150g145g144g139g150g148g139g142g135g3g135g150g3g146g151g148g139g136g139g133g131g150g139g145g144g3g146g131g148g3g22g19g8g3g134g139g149g146g135g148g
11、149g139g152g135g3g486g3g7g145g144g144g177g135g149g3g134g135g3g152g131g142g139g134g131g150g139g145g144g3g134g135g3g142g131g3g143g177g150g138g145g134g135g3g143g145g134g151g142g131g139g148g135g3g20g151g8g6g138g8g21g22g3g3 g19g136g142g131g144g156g142g139g133g138g135g3g15g135g132g135g144g149g143g139g150g
12、150g135g142g3g486g3g16g151g142g150g139g152g135g148g136g131g138g148g135g144g3g156g151g148g3g5g135g149g150g139g143g143g151g144g137g3g152g145g144g3g19g135g149g150g139g156g139g134g148g242g133g141g149g150g161g144g134g135g144g3g143g139g150g3g10g6g486g3g145g134g135g148g3g15g6g486g25g135g148g136g131g138g148
13、g135g144g3g144g131g133g138g3g4g133g135g150g145g144g139g150g148g139g142g3g8g154g150g148g131g141g150g139g145g144g512g25g135g148g150g135g139g142g151g144g137g3g151g144g134g3g21g135g139g144g139g137g151g144g137g3g143g139g150g3g134g139g149g146g135g148g149g139g152g135g148g3g22g19g8g3g486g3g25g131g142g139g13
14、4g139g135g148g151g144g137g149g134g131g150g135g144g3g134g135g149g3g143g145g134g151g142g131g148g135g144g3g20g151g8g6g138g8g21g22g486g25g135g148g136g131g138g148g135g144g149g3g3g3g23g138g139g149g3g23g135g133g138g144g139g133g131g142g3g21g135g146g145g148g150g3g153g131g149g3g131g146g146g148g145g152g135g134
15、g3g132g155g3g6g8g17g3g145g144g3g885g3g16g131g148g133g138g3g884g882g883g889g484g3g12g150g3g138g131g149g3g132g135g135g144g3g134g148g131g153g144g3g151g146g3g132g155g3g150g138g135g3g23g135g133g138g144g139g133g131g142g3g6g145g143g143g139g150g150g135g135g3g6g8g17g512g23g6g3g884g889g887g484g3g3g6g8g17g3g14
16、3g135g143g132g135g148g149g3g131g148g135g3g150g138g135g3g144g131g150g139g145g144g131g142g3g149g150g131g144g134g131g148g134g149g3g132g145g134g139g135g149g3g145g136g3g4g151g149g150g148g139g131g481g3g5g135g142g137g139g151g143g481g3g5g151g142g137g131g148g139g131g481g3g6g148g145g131g150g139g131g481g3g6g15
17、5g146g148g151g149g481g3g6g156g135g133g138g3g21g135g146g151g132g142g139g133g481g3g7g135g144g143g131g148g141g481g3g8g149g150g145g144g139g131g481g3g9g139g144g142g131g144g134g481g3g9g145g148g143g135g148g3g28g151g137g145g149g142g131g152g3g21g135g146g151g132g142g139g133g3g145g136g3g16g131g133g135g134g145g
18、144g139g131g481g3g9g148g131g144g133g135g481g3g10g135g148g143g131g144g155g481g3g10g148g135g135g133g135g481g3g11g151g144g137g131g148g155g481g3g12g133g135g142g131g144g134g481g3g12g148g135g142g131g144g134g481g3g12g150g131g142g155g481g3g15g131g150g152g139g131g481g3g15g139g150g138g151g131g144g139g131g481g
19、3g15g151g154g135g143g132g145g151g148g137g481g3g16g131g142g150g131g481g3g17g135g150g138g135g148g142g131g144g134g149g481g3g17g145g148g153g131g155g481g3g19g145g142g131g144g134g481g3g19g145g148g150g151g137g131g142g481g3g21g145g143g131g144g139g131g481g3g22g135g148g132g139g131g481g3g22g142g145g152g131g141
20、g139g131g481g3g22g142g145g152g135g144g139g131g481g3g22g146g131g139g144g481g3g22g153g135g134g135g144g481g3g22g153g139g150g156g135g148g142g131g144g134g481g3g23g151g148g141g135g155g3g131g144g134g3g24g144g139g150g135g134g3g14g139g144g137g134g145g143g484g3g3g3g3g3g8g24g21g18g19g8g4g17g3g6g18g16g16g12g23g
21、23g8g8g3g9g18g21g3g22g23g4g17g7g4g21g7g12g29g4g23g12g18g17g3g6g18g16g12g23g50g3g8g24g21g18g19g50g8g17g3g7g8g3g17g18g21g16g4g15g12g22g4g23g12g18g17g3g8g24g21g18g19g34g12g22g6g11g8g22g3g14g18g16g12g23g8g8g3g9g111g21g3g17g18g21g16g24g17g10g3g3g3g3CEN-CENELECg3Management Centre: Avenue Marnix 17, B-1000
22、 Brussels g825g3g884g882g883g889g3g6g8g17g3 g4g142g142g3g148g139g137g138g150g149g3g145g136g3g135g154g146g142g145g139g150g131g150g139g145g144g3g139g144g3g131g144g155g3g136g145g148g143g3g131g144g134g3g132g155g3g131g144g155g3g143g135g131g144g149g3g148g135g149g135g148g152g135g134g3g153g145g148g142g134g1
23、53g139g134g135g3g136g145g148g3g6g8g17g3g144g131g150g139g145g144g131g142g3g16g135g143g132g135g148g149g484g3g21g135g136g484g3g17g145g484g3g6g8g17g512g23g21g3g883g889g882g888g885g483g884g882g883g889g3g8PD CEN/TR 17063:2017CEN/TR 17063:2017 (E) 2 Contents Page European foreword . 3 1 Scope 3 2 Normative
24、 references 4 3 General 4 Bibliography . 86 PD CEN/TR 17063:2017g6g8g17g512g23g21g3g883g889g882g888g885g483g884g882g883g889g3g525g8g5262CEN/TR 17063:2017 (E) 3 European foreword This document (CEN/TR 17063:2017) has been prepared by Technical Committee CEN/TC 275 “Food analysis - Horizontal methods”
25、, the secretariat of which is held by DIN. 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 any or all such patent rights. PD CEN/TR 17063:2017PD CEN/TR 17063:2017g6g8g17g512g23g21g
26、3g883g889g882g888g885g483g884g882g883g889g3g525g8g5263CEN/TR 17063:2017 (E) 4 1 Scope This Technical Report lists the validation data which were obtained with EN 15662:2008 and prEN 15662:2016 in interlaboratory tests and in single laboratory method validation studies. 2 Normative references Not app
27、licable. 3 General When the applicability of these validation data in Table 1 is considered, the most important difference between EN 15662:2008 and prEN 15662:2016 is the duration of first extraction. This first extraction was extended from 1 min to 15 min. It is assumed that the extended extractio
28、n does not result in reduced recoveries. Instable pesticides are the only exception. Well known examples are the losses of chlorothalonil in extracts of Allium, the oxidation of Malathion in cereals after addition of water and the degradation of thiram in plant homogenates. Furthermore, in plant hom
29、ogenates the formation of carbofuran from carbosulfan or benfuracarb and the formation of carbendazim from benomyl or thiophanate-methyl can be observed. Finally, several pesticides of the sulfonyl urea group are known for fast hydrolysis at pH conditions used within QuEChERS. Validity of the method
30、 has been supposed to be confirmed for any specific commodity/pesticide combination if at least two laboratories conducted independently validation studies with the same matrix at two identical fortification levels with at least five replicates per level and obtained a recovery between 70 % and 120
31、%. Furthermore, the relative standard deviation had to be below or equal 20 % for both spiking levels in each laboratory. PD CEN/TR 17063:2017g6g8g17g512g23g21g3g883g889g882g888g885g483g884g882g883g889g3g525g8g5264CEN/TR17063:2017 (E)5Table1 Precisiondata andresults of recoverytests (approximately50
32、.000individual results)Analyte /CAS-No.MatrixgroupMatrixExtraction moduleClean-upGC/LCLevelaRecoveryRSDb% ncLabsd2.4-DHigh watercontentCucumberE1 C0 LC 0,01100 12,645 7 94-75-7 High watercontentCucumberE1 C0 LC 0,1 95 12 62 9 High watercontentAppleE1 C2 LC 0,0279 19,314 1 AcidicLemonE2aC0 LC0,01103
33、7,6 35 6 AcidicLemonE2aC0 LC0,1 99 7,9 35 6 AcidicLemonE2aC1 LC0,00597 3,8 51AcidicLemonE2aC1 LC0,1 89 8,7 15 3 High watercontentBananaE3aC0 LC 0,025102 11 6 1 Sugar containingGrapes, driedE4 C0 LC 0,0196 15 25 5 Sugar containingGrapes,driedE4 C0LC0,1 96 9,4 35 6 Sugar containingHoneyE5 C2 LC 0,0283
34、 9 5 1 Dry (cereals, dry pulses)WheatflourE5 C1 LC 0,0193 9,3 10 2 Dry (cereals, dry pulses)WheatflourE5 C1 LC 0,1 96 6,6 15 2Dry (cereals, dry pulses)WheatflourE5 C0 LC 0,0194 12 28 5 Dry (cereals,dry pulses)Wheat flour E5C0LC 0,1949265AcephateHigh watercontentCucumberE1 C2 LC 0,0182 12,620 3 30560
35、-19-1High watercontentCucumberE1 C2 LC 0,1 87 8,4 26 4 AcidicLemonE2aC2 LC0,0190 7,9 10 2 AcidicLemonE2aC2 LC0,1 89 11,115 3 AcidicLemonE2aC1 LC0,00579 1,6 51Sugar containingGrapes, driedE4 C2 LC 0,0182 7,9 15 3 Sugar containingGrapes,driedE4 C2LC0,1 81 7,2 15 3 Dry (cereals, dry pulses)WheatflourE5
36、 C1+C3aLC 0,0181 12,815 3 Dry (cereals, dry pulses)WheatflourE5 C1+C3aLC 0,1 81 6 15 3Dry (cereals,dry pulses)Wheat flour E5C1LC 0,1778,151AcetamipridHigh watercontentAppleE1 C2 LC 0,02598 7,1 46 8 PD CEN/TR 17063:2017PD CEN/TR 17063:2017g6g8g17g512g23g21g3g883g889g882g888g885g483g884g882g883g889g3g
37、525g8g5265CEN/TR17063:2017 (E)6 Analyte /CAS-No.MatrixgroupMatrixExtraction moduleClean-upGC/LCLevelaRecoveryRSDb% ncLabsd135410-20-7High watercontentAppleE1 C2 LC 0,2599 5 40 8High watercontentCucumberE1 C2 LC 0,0196 5,6 35 6 High watercontentCucumberE1 C2 LC 0,1 98 5,9 37 6 High watercontentLettuc
38、e,headE1 C2 LC 0,02597 6,5 37 7 High watercontentLettuce,headE1 C2 LC 0,2597 7,5 45 9 AcidicOrangeE1 C2 LC0,02596 7,5 32 6 AcidicOrangeE1 C2 LC0,2597 3,6 35 7 AcidicLemonE2aC2 LC0,0197 8,4 30 6 AcidicLemonE2aC2 LC0,1 96 8,4 30 6 AcidicLemonE2aC1 LC0,005102 17,251AcidicLemonE2aC1 LC0,1 99 2,9 51Sugar
39、 containingGrapes, driedE4 C2 LC 0,0197 6,7 20 4 Sugar containingGrapes,driedE4 C2LC0,1 99 6,3 25 5 Sugar containingHoneyE5 C2 LC 0,0194 4,2 51Sugar containingHoneyE5 C2 LC 0,1 96 4,6 51Dry (cereals, dry pulses)WheatflourE5 C1+C3aLC 0,0199 6,8 20 4 Dry (cereals, dry pulses)WheatflourE5 C1+C3aLC 0,1
40、97 4,9 15 3 Dry (cereals, dry pulses)WheatflourE5 C3aLC 0,1 95 9,1 10 2 Fatty, wet (oily fruits)Avocado E6 C4 LC 0,0199 2,8 51Fatty, wet (oily fruits)Avocado E6 C4 LC0,1 103 3,5 51AcrinathrinHigh watercontentCucumberE1 C2 GC 0,0298 10,350 6 101007-06-1High watercontentCucumberE1 C2 GC 0,1 92 6,3 26
41、4 AcidicLemonE2aC2 GC 0,0298 7,9 40 4 AcidicLemonE2aC2 GC 0,1 85 8,1 20 4 Sugar containingGrapes, driedE4 C2 GC 0,0299 8 46 5Sugar containingGrapes, driedE4 C2 GC 0,1 90 11,428 5 Dry (cereals, dry pulses)WheatflourE5 C1+C3aGC 0,0297 9,2 21 4 Dry (cereals, dry pulses)WheatflourE5 C1+C3aGC 0,1 95 12,9
42、16 3 PD CEN/TR 17063:2017PD CEN/TR 17063:2017g6g8g17g512g23g21g3g883g889g882g888g885g483g884g882g883g889g3g525g8g5266CEN/TR17063:2017 (E)7Analyte /CAS-No.MatrixgroupMatrixExtraction moduleClean-upGC/LCLevelaRecoveryRSDb% ncLabsdAldicarb High watercontentCucumberE1 C2 LC 0,0197 7,1 25 4 116-06-3 High
43、 watercontentCucumberE1 C2 LC 0,1 93 12,126 4 AcidicLemonE2aC2 LC0,0196 7,3 15 3 AcidicLemonE2aC2 LC0,1 100 5,6 15 3 AcidicLemonE2aC1 LC0,00592 2,1 51Sugar containingGrapes, driedE4 C2 LC 0,0198 9,6 21 4 Sugar containingGrapes,driedE4 C2LC0,1 95 9,6 21 4 Dry (cereals, dry pulses)WheatflourE5 C1+C3aL
44、C 0,01100 7,4 15 3 Dry (cereals, dry pulses)WheatflourE5 C1+C3aLC 0,1 97 5,6 15 3 AvermectinB1aHigh watercontentCucumberE1 C2 LC 0,0188 17,115 3 65195-55-3High watercontentCucumberE1 C2 LC 0,1 87 10,115 3 AcidicLemonE2aC2 LC0,0186 12,215 3 AcidicLemonE2aC2 LC0,1 96 13 25 5 AcidicLemonE2aC1 LC0,1 94
45、1,1 51Sugar containingGrapes, driedE4 C2 LC 0,0194 17,710 2 Sugar containingGrapes,driedE4 C2LC0,1 100 8,7 15 3 Dry (cereals, dry pulses)WheatflourE5 C1+C3aLC 0,0199 16,810 2 Dry (cereals, dry pulses)WheatflourE5 C1+C3aLC 0,1 96 12,115 3 Dry (cereals, dry pulses)WheatflourE5 C1 LC 0,1 104 5,7 10 1 A
46、zinphos-methylHigh watercontentCucumberE1 C2 LC 0,0195 10,436 6 86-50-0 High watercontentCucumberE1 C2 LC 0,1 97 9,5 36 6 AcidicLemonE2aC2 LC0,01100 12,120 4 Acidic LemonE2aC2 LC 0,1 105 8,4 20 4 AcidicLemonE2aC1 LC0,1 94 8,6 10 2 Sugar containingGrapes, driedE4 C2 LC 0,01102 9,2 21 4 Sugar containi
47、ngGrapes, driedE4 C2 LC 0,1 98 10,926 5 PD CEN/TR 17063:2017PD CEN/TR 17063:2017g6g8g17g512g23g21g3g883g889g882g888g885g483g884g882g883g889g3g525g8g5267CEN/TR17063:2017 (E)8 Analyte /CAS-No.MatrixgroupMatrixExtraction moduleClean-upGC/LCLevelaRecoveryRSDb% ncLabsdDry (cereals, dry pulses)WheatflourE
48、5 C3aLC 0,0198 6,5 15 3 Dry (cereals, dry pulses)WheatflourE5 C3aLC 0,1 98 11,820 4 AzoxystrobinHigh watercontentCucumberE1 C2 LC 0,0196 5,2 30 5 131860-33-8High watercontentCucumberE1 C2 LC 0,1 99 5,4 30 5 AcidicLemonE2aC2 LC0,01102 5,8 20 4 AcidicLemonE2aC2 LC0,1 95 5,2 20 4 Sugar containingGrapes
49、, driedE4 C2 LC 0,01102 5,7 20 4 Sugar containingGrapes,driedE4 C2LC0,1 99 4,3 20 4 Sugar containingHoneyE5 C2 LC 0,0199 2,7 51Sugar containingHoneyE5 C2 LC 0,1 94 4,6 51Dry (cereals, dry pulses)WheatflourE5 C1+C3aLC 0,0195 7,7 15 3 Dry (cereals, dry pulses)WheatflourE5 C1+C3aLC 0,1 99 3,4 15 3 Fatty, wet (oily fruits)Avocado E6 C4 LC 0,0195 3,7 51Fatty, wet (oily fruits)Avocado E6 C4 LC0,1 107 351Dry (spices,herbs,tea)Tea, blackE7 C3bLC 0,0579 10,161Dry (spices,herbs,tea)Tea, blackE7 C3bLC 0,5 81 7,6 61Benalaxyl High water contentCucumberE1 C2 LC 0,0198 8,2 51 9 71626-11-4High
