CEN/TR 17063:2017

Foods of plant origin - Multimethod for the determination of pesticide residues using GC- or LC-based analysis following acetonitrile extraction/partitioning and cleanup by dispersive SPE - Validation data of the modular QuEChERS-method

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.

Pflanzliche Lebensmittel - Multiverfahren zur Bestimmung von Pestizidrückständen mit GC- oder LC-Verfahren nach Acetonitril-Extraktion/-Verteilung und Reinigung mit dispersiver SPE - Validierungsdaten des modularen QuEChERS-Verfahrens

Dieser Technische Bericht listet die Validierungsdaten auf, die mit EN 15662:2008 und prEN 15662:2017N1) in Ringversuchen und in Validierungen einzelner Labore erhalten wurden

Aliments d'origine végétale - Multiméthode de détermination des résidus de pesticides par analyse CG ou CL après extraction/partition avec de l'acétonitrile et purification par SPE dispersive - Données de validation de la méthode modulaire QuEChERS

Le présent Rapport technique répertorie les données de validation obtenues avec l’EN 15662:2008 et la prEN 15662:2016 au cours d’essais interlaboratoires et d’études de validation de la méthode en laboratoire.

Živila rastlinskega izvora - Metode za določevanje ostankov pesticidov z uporabo analiz, osnovanih na plinski ali tekočinski kromatografiji po acetonitrilni ekstrakciji/ločevanju in čiščenju z disperzivnim SPE - Validacijski podatki modularne metode QuEChERS

To tehnično poročilo navaja podatke o validaciji, pridobljene v skladu s standardoma EN 15662:2008 in prEN 15662:2016 pri medlaboratorijskih preskusih in validativnih študijah na podlagi enotne laboratorijske metode.

General Information

• Status: Published
• Publication Date: 14-Mar-2017
• ICS: 67.050 - General methods of tests and analysis for food products
• Technical Committee: CEN/TC 275 - Food analysis - Horizontal methods
• Drafting Committee: CEN/TC 275/WG 3 - Pesticides and PCB's in foods of animal origin
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 15-Mar-2017
• Due Date: 09-Jul-2017
• Completion Date: 15-Mar-2017
• Directive: 882/2004 - Regulation (EC) No 882/2004 of the European Parliament and of the Council of 29 April 2004 onofficial controls performed to ensure the verification of compliance with feed and food law, animal health and animal welfare rules
• Ref Project: SIST-TP CEN/TR 17063:2017 - Foods of plant origin - Multimethod for the determination of pesticide residues using GC- or LC-based analysis following acetonitrile extraction/partitioning and cleanup by dispersive SPE - Validation data of the modular QuEChERS-method

Standards Content (Sample)

SLOVENSKI STANDARD
01-maj-2017
äLYLODUDVWOLQVNHJDL]YRUD0HWRGH]DGRORþHYDQMHRVWDQNRYSHVWLFLGRY]XSRUDER
DQDOL]RVQRYDQLKQDSOLQVNLDOLWHNRþLQVNLNURPDWRJUDILMLSRDFHWRQLWULOQL
HNVWUDNFLMLORþHYDQMXLQþLãþHQMX]GLVSHU]LYQLP63(9DOLGDFLMVNLSRGDWNL
PRGXODUQHPHWRGH4X(&K(56
Foods of plant origin - Multimethod for the determination of pesticide residues using GC-
or LC-based analysis following acetonitrile extraction/partitioning and cleanup by
dispersive SPE - Validation data of the modular QuEChERS-method
Pflanzliche Lebensmittel - Multiverfahren zur Bestimmung von Pestizidrückständen mit
GC- oder LC-Verfahren nach Acetonitril Extraktion/Verteilung und Reinigung mit
dispersiver SPE - Validierungsdaten des modularen QuEChERS-Verfahrens
Aliments d'origine végétale - Méthodes multiples de détermination des résidus de
pesticides par analyse CG ou CL après extraction/partition avec de l'acétonitrile et
purification par SPE dispersive - Données de validation de la méthode modulaire
QuEChERS
Ta slovenski standard je istoveten z: CEN/TR 17063:2017
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

CEN/TR 17063
TECHNICAL REPORT
RAPPORT TECHNIQUE
March 2017
TECHNISCHER BERICHT
ICS 67.050
English Version
Foods of plant origin - Multimethod for the determination
of pesticide residues using GC- or LC-based analysis
following acetonitrile extraction/partitioning and cleanup
by dispersive SPE - Validation data of the modular
QuEChERS-method
Aliments d'origine végétale - Méthodes multiples de Pflanzliche Lebensmittel - Multiverfahren zur
détermination des résidus de pesticides par analyse CG Bestimmung von Pestizidrückständen mit GC- oder LC-
ou CL après extraction/partition avec de l'acétonitrile Verfahren nach Acetonitril Extraktion/Verteilung und
et purification par SPE dispersive - Données de Reinigung mit dispersiver SPE - Validierungsdaten des
validation de la méthode modulaire QuEChERS modularen QuEChERS-Verfahrens

This Technical Report was approved by CEN on 3 March 2017. It has been drawn up by the Technical Committee CEN/TC 275.

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, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2017 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 17063:2017 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
1 Scope . 3
2 Normative references . 4
3 General . 4
Bibliography . 86
European foreword
This document (CEN/TR 17063:2017) has been prepared by Technical Committee CEN/TC 275 “Food
analysis - Horizontal methods”, 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.
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 applicable.
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 extraction 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 homogenates 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 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 %. Furthermore, the relative standard deviation had to be below or equal 20 %
for both spiking levels in each laboratory.
Table 1 — Precision data and results of recovery tests (approximately 50.000 individual results)
a b c d
Analyte / CAS-No. Matrix group Matrix Extraction Clean-up GC/LC Level Recovery RSD n Labs
module
%
2.4-D High water content Cucumber E1 C0 LC 0,01 100 12,6 45 7
94-75-7 High water content Cucumber E1 C0 LC 0,1 95 12 62 9
High water content Apple E1 C2 LC 0,02 79 19,3 14 1
Acidic Lemon E2a C0 LC 0,01 103 7,6 35 6
Acidic Lemon E2a C0 LC 0,1 99 7,9 35 6
Acidic Lemon E2a C1 LC 0,005 97 3,8 5 1
Acidic Lemon E2a C1 LC 0,1 89 8,7 15 3
High water content Banana E3a C0 LC 0,025 102 11 6 1
Sugar containing Grapes, dried E4 C0 LC 0,01 96 15 25 5
Sugar containing Grapes, dried E4 C0 LC 0,1 96 9,4 35 6
Sugar containing Honey E5 C2 LC 0,02 83 9 5 1
Dry (cereals, dry pulses) Wheat flour E5 C1 LC 0,01 93 9,3 10 2
Dry (cereals, dry pulses) Wheat flour E5 C1 LC 0,1 96 6,6 15 2
Dry (cereals, dry pulses) Wheat flour E5 C0 LC 0,01 94 12 28 5
Dry (cereals, dry pulses) Wheat flour E5 C0 LC 0,1 94 9 26 5

Acephate High water content Cucumber E1 C2 LC 0,01 82 12,6 20 3
30560-19-1 High water content Cucumber E1 C2 LC 0,1 87 8,4 26 4
Acidic Lemon E2a C2 LC 0,01 90 7,9 10 2
Acidic Lemon E2a C2 LC 0,1 89 11,1 15 3
Acidic Lemon E2a C1 LC 0,005 79 1,6 5 1
Sugar containing Grapes, dried E4 C2 LC 0,01 82 7,9 15 3
Sugar containing Grapes, dried E4 C2 LC 0,1 81 7,2 15 3
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a LC 0,01 81 12,8 15 3
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a LC 0,1 81 6 15 3
Dry (cereals, dry pulses) Wheat flour E5 C1 LC 0,1 77 8,1 5 1

Acetamiprid High water content Apple E1 C2 LC 0,025 98 7,1 46 8
a b c d
Analyte / CAS-No. Matrix group Matrix Extraction Clean-up GC/LC Level Recovery RSD n Labs
module
%
135410-20-7 High water content Apple E1 C2 LC 0,25 99 5 40 8
High water content Cucumber E1 C2 LC 0,01 96 5,6 35 6
High water content Cucumber E1 C2 LC 0,1 98 5,9 37 6
High water content Lettuce, head E1 C2 LC 0,025 97 6,5 37 7
High water content Lettuce, head E1 C2 LC 0,25 97 7,5 45 9
Acidic Orange E1 C2 LC 0,025 96 7,5 32 6
Acidic Orange E1 C2 LC 0,25 97 3,6 35 7
Acidic Lemon E2a C2 LC 0,01 97 8,4 30 6
Acidic Lemon E2a C2 LC 0,1 96 8,4 30 6
Acidic Lemon E2a C1 LC 0,005 102 17,2 5 1
Acidic Lemon E2a C1 LC 0,1 99 2,9 5 1
Sugar containing Grapes, dried E4 C2 LC 0,01 97 6,7 20 4
Sugar containing Grapes, dried E4 C2 LC 0,1 99 6,3 25 5
Sugar containing Honey E5 C2 LC 0,01 94 4,2 5 1
Sugar containing Honey E5 C2 LC 0,1 96 4,6 5 1
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a LC 0,01 99 6,8 20 4
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a LC 0,1 97 4,9 15 3
Dry (cereals, dry pulses) Wheat flour E5 C3a LC 0,1 95 9,1 10 2
Fatty, wet (oily fruits) Avocado E6 C4 LC 0,01 99 2,8 5 1
Fatty, wet (oily fruits) Avocado E6 C4 LC 0,1 103 3,5 5 1

Acrinathrin High water content Cucumber E1 C2 GC 0,02 98 10,3 50 6
101007-06-1 High water content Cucumber E1 C2 GC 0,1 92 6,3 26 4
Acidic Lemon E2a C2 GC 0,02 98 7,9 40 4
Acidic Lemon E2a C2 GC 0,1 85 8,1 20 4
Sugar containing Grapes, dried E4 C2 GC 0,02 99 8 46 5
Sugar containing Grapes, dried E4 C2 GC 0,1 90 11,4 28 5
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a GC 0,02 97 9,2 21 4
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a GC 0,1 95 12,9 16 3
a b c d
Analyte / CAS-No. Matrix group Matrix Extraction Clean-up GC/LC Level Recovery RSD n Labs
module
%
Aldicarb High water content Cucumber E1 C2 LC 0,01 97 7,1 25 4
116-06-3 High water content Cucumber E1 C2 LC 0,1 93 12,1 26 4
Acidic Lemon E2a C2 LC 0,01 96 7,3 15 3
Acidic Lemon E2a C2 LC 0,1 100 5,6 15 3
Acidic Lemon E2a C1 LC 0,005 92 2,1 5 1
Sugar containing Grapes, dried E4 C2 LC 0,01 98 9,6 21 4
Sugar containing Grapes, dried E4 C2 LC 0,1 95 9,6 21 4
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a LC 0,01 100 7,4 15 3
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a LC 0,1 97 5,6 15 3

Avermectin B1a High water content Cucumber E1 C2 LC 0,01 88 17,1 15 3
65195-55-3 High water content Cucumber E1 C2 LC 0,1 87 10,1 15 3
Acidic Lemon E2a C2 LC 0,01 86 12,2 15 3
Acidic Lemon E2a C2 LC 0,1 96 13 25 5
Acidic Lemon E2a C1 LC 0,1 94 1,1 5 1
Sugar containing Grapes, dried E4 C2 LC 0,01 94 17,7 10 2
Sugar containing Grapes, dried E4 C2 LC 0,1 100 8,7 15 3
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a LC 0,01 99 16,8 10 2
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a LC 0,1 96 12,1 15 3
Dry (cereals, dry pulses) Wheat flour E5 C1 LC 0,1 104 5,7 10 1

Azinphos-methyl High water content Cucumber E1 C2 LC 0,01 95 10,4 36 6
86-50-0 High water content Cucumber E1 C2 LC 0,1 97 9,5 36 6
Acidic Lemon E2a C2 LC 0,01 100 12,1 20 4
Acidic Lemon E2a C2 LC 0,1 105 8,4 20 4
Acidic Lemon E2a C1 LC 0,1 94 8,6 10 2
Sugar containing Grapes, dried E4 C2 LC 0,01 102 9,2 21 4
Sugar containing Grapes, dried E4 C2 LC 0,1 98 10,9 26 5
a b c d
Analyte / CAS-No. Matrix group Matrix Extraction Clean-up GC/LC Level Recovery RSD n Labs
module
%
Dry (cereals, dry pulses) Wheat flour E5 C3a LC 0,01 98 6,5 15 3
Dry (cereals, dry pulses) Wheat flour E5 C3a LC 0,1 98 11,8 20 4

Azoxystrobin High water content Cucumber E1 C2 LC 0,01 96 5,2 30 5
131860-33-8 High water content Cucumber E1 C2 LC 0,1 99 5,4 30 5
Acidic Lemon E2a C2 LC 0,01 102 5,8 20 4
Acidic Lemon E2a C2 LC 0,1 95 5,2 20 4
Sugar containing Grapes, dried E4 C2 LC 0,01 102 5,7 20 4
Sugar containing Grapes, dried E4 C2 LC 0,1 99 4,3 20 4
Sugar containing Honey E5 C2 LC 0,01 99 2,7 5 1
Sugar containing Honey E5 C2 LC 0,1 94 4,6 5 1
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a LC 0,01 95 7,7 15 3
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a LC 0,1 99 3,4 15 3
Fatty, wet (oily fruits) Avocado E6 C4 LC 0,01 95 3,7 5 1
Fatty, wet (oily fruits) Avocado E6 C4 LC 0,1 107 3 5 1
Dry (spices, herbs, tea) Tea, black E7 C3b LC 0,05 79 10,1 6 1
Dry (spices, herbs, tea) Tea, black E7 C3b LC 0,5 81 7,6 6 1

Benalaxyl High water content Cucumber E1 C2 LC 0,01 98 8,2 51 9
71626-11-4 High water content Cucumber E1 C2 LC 0,1 98 9,1 51 9
Acidic Lemon E2a C2 LC 0,01 98 7,1 41 8
Acidic Lemon E2a C2 LC 0,1 100 6 46 9
Acidic Lemon E2a C1 LC 0,005 95 8,3 5 1
Sugar containing Grapes, dried E4 C2 LC 0,01 97 5,6 41 8
Sugar containing Grapes, dried E4 C2 LC 0,1 100 5,4 41 8
Dry (cereals, dry pulses) Wheat flour E5 C3a LC 0,01 100 7,2 20 4
Dry (cereals, dry pulses) Wheat flour E5 C3a LC 0,1 101 6,5 25 5
Fatty, wet (oily fruits) Avocado E6 C0 LC 0,1 101 4,2 5 1
Dry (spices, herbs, tea) Tea, black E7 C3b LC 0,05 84 6,3 6 1
a b c d
Analyte / CAS-No. Matrix group Matrix Extraction Clean-up GC/LC Level Recovery RSD n Labs
module
%
Dry (spices, herbs, tea) Tea, black E7 C3b LC 0,5 85 4,3 6 1

Bifenthrin High water content Cucumber E1 C2 GC 0,02 95 7,8 72 9
82657-04-3 High water content Cucumber E1 C2 GC 0,05 101 7,4 55 8
High water content Cucumber E1 C2 GC 0,1 99 8,5 63 7
Acidic Lemon E2a C2 GC 0,02 100 4,1 40 3
Acidic Lemon E2a C2 GC 0,05 103 5,6 34 5
Acidic Lemon E2a C2 GC 0,1 106 8,6 49 6
Acidic Lemon E2a C1 GC 0,005 105 2,4 5 1
Acidic Lemon E2a C1 GC 0,02 112 1,2 5 1
Sugar containing Grapes, dried E4 C2 GC 0,02 98 6,7 46 4
Sugar containing Grapes, dried E4 C2 GC 0,05 98 6,1 26 4
Sugar containing Grapes, dried E4 C2 GC 0,1 102 6,3 48 6
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a GC 0,02 95 8,1 36 6
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a GC 0,05 102 6,5 36 6
Dry (cereals, dry pulses) Wheat flour E5 C1+C3a GC 0,1 106 3,7 26 5

Biphenyl High water content Cucumber E1 C2 GC 0,02 94 9,2 31 6
92-52-4 High water conte
...