prEN 18082
(Main)Foods of animal origin - Multimethod for the determination of pesticide residues using LC-based analysis following acetonitrile extraction/partitioning and clean-up by dispersive SPE
Foods of animal origin - Multimethod for the determination of pesticide residues using LC-based analysis following acetonitrile extraction/partitioning and clean-up by dispersive SPE
This document specifies a method for the analysis of pesticide residues in foods of animal origin with a fat content of up to approximatively 10 %, such as meat, egg or milk by LC-MS/MS. Because of the low material requirements for miniaturized processing and the few work steps, the process is particularly time and cost-saving with high reliability and effectiveness. The method has been collaboratively studied on a number of commodity/pesticide combinations. Precision data are summarized in Table B.1. Guidelines for calibration are outlined in CEN/TS 17061.
Tierische Lebensmittel - Multiverfahren zur Bestimmung von Pestizidrückständen mit LC nach Acetonitril-Extraktion/Verteilung und Reinigung mit dispersiver SPE
Dieses Dokument legt ein Verfahren für die Analyse von Pestizidrückständen in Lebensmitteln tierischer Herkunft mit einem Fettgehalt von bis zu ca. 10 %, wie z. B. Fleisch, Eier oder Milch, mittels LC-MS/MS fest. Aufgrund der geringen Materialanforderungen für die miniaturisierte Verarbeitung und der wenigen Arbeitsschritte ist das Verfahren besonders zeit- und kostensparend bei hoher Zuverlässigkeit und Effektivität. Das Verfahren wurde im Ringversuch mit einer Reihe an Erzeugnis-/Pestizidkombinationen geprüft. Die Präzisionsdaten sind in Tabelle B.1 zusammengefasst. Eine Anleitung zur Kalibrierung ist in CEN/TS 17061 angegeben.
Aliments d'origine animale - Multiméthode de détermination des résidus de pesticides par analyse CL après extraction/partition avec de l'acétonitrile et purification par SPE dispersive
Le présent document décrit une méthode d'analyse CL-SM/SM des résidus de pesticides dans les aliments d'origine animale dont la teneur en matière grasse est inférieure ou égale à 10 % environ, tels que la viande, les œufs ou le lait. En raison des faibles besoins en produits pour la transformation miniaturisée et du nombre réduit d'étapes de travail, le processus est particulièrement économe en temps et en argent, tout en offrant une fiabilité et une efficacité élevées. La méthode a fait l'objet d'un essai interlaboratoires portant sur plusieurs combinaisons denrée/pesticide. Les données de fidélité sont résumées dans le Tableau B.1. Les lignes directrices relatives à l'étalonnage sont données dans la CEN/TS 17061.
Živila živalskega izvora - Multimetoda za določanje ostankov pesticidov z uporabo LC-analize po acetonitrilni ekstrakciji/delitvi in čiščenju z disperzijsko SPE
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-julij-2024
Živila živalskega izvora - Multimetoda za določanje ostankov pesticidov z uporabo
LC-analize po acetonitrilni ekstrakciji/delitvi in čiščenju z disperzijsko SPE
Foods of animal origin - Multimethod for the determination of pesticide residues using
LC-based analysis following acetonitrile extraction/partitioning and clean-up by
dispersive SPE
Tierische Lebensmittel - Multiverfahren zur Bestimmung von Pestizidrückständen mit LC
nach Acetonitril-Extraktion/Verteilung und Reinigung mit dispersiver SPE
Ta slovenski standard je istoveten z: prEN 18082
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
67.120.01 Živila živalskega izvora na Animal produce in general
splošno
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
DRAFT
EUROPEAN STANDARD
NORME EUROPÉENNE
EUROPÄISCHE NORM
May 2024
ICS 67.050; 67.120.01
English Version
Foods of animal origin - Multimethod for the
determination of pesticide residues using LC-based
analysis following acetonitrile extraction/partitioning and
clean-up by dispersive SPE
Tierische Lebensmittel - Multiverfahren zur
Bestimmung von Pestizidrückständen mit LC nach
Acetonitril-Extraktion/Verteilung und Reinigung mit
dispersiver SPE
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 275.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 18082:2024 E
worldwide for CEN national Members.
Contents Page
European foreword . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 5
5 Preparation and storage of the samples . 5
5.1 General. 5
5.2 Laboratory sample . 6
5.3 Partly-prepared test sample . 6
5.4 Test sample . 6
5.5 Test portion . 6
6 Procedure . 6
7 Evaluation of results . 7
7.1 Identification and quantification . 7
7.2 Calibration . 8
7.3 Calculation of residue concentration. 8
7.4 Validity of the method . 9
8 Precision . 11
9 Test report . 11
Annex A (informative) Description of modules . 12
A.1 Reagents used in extraction (E) and clean-up (C) modules . 12
A.2 Apparatus used in extraction (E) and clean-up (C) modules . 13
A.3 Description of extraction (E) module . 14
A.3.1 Module E: Extraction of a 5 g test portion with additional water using acetonitrile . 14
A.4 Description of clean-up (C) modules . 16
A.4.1 Module C1: Clean-up by freezing-out of co-extracted fat . 16
A.4.2 Module C2: Clean-up by dispersive SPE with amine sorbent (PSA) . 17
A.5 Description of detection (D) modules . 18
A.5.1 Module D: Determination using liquid chromatography with mass spectrometric detection
(LC-MS) . 18
A.6 Description of quantification (Q) options . 22
A.6.1 Option Q1: Quantification using external standards in solvent . 22
A.6.2 Option Q2: Quantification using external standards in matrix . 22
A.6.3 Option Q3: Quantification using a procedural internal standard and standards in solvent
............................................................................................................................................................................. 23
A.6.4 Option Q4: Quantification using standard addition to the final extract . 23
A.6.5 Option Q5: Quantification using a procedural internal standard and standards in matrix or
isotope-labelled internal standards . 24
A.6.6 Option Q6: Quantification using standard addition to the sample . 25
A.6.7 Option Q7: Quantification by calibration of the entire procedure . 25
Annex B (informative) Complementary information . 26
B.1 General . 26
B.2 Preparation of the buffer-salt mixture (A.1.8) . 26
B.3 Reagents for clean-up. 26
B.4 Prolongation of extraction time . 26
B.5 Working with internal standards . 26
B.6 Scaling . 26
B.7 Validation data . 26
Annex C (informative) Abbreviations and symbols. 42
Bibliography . 44
European foreword
This document (prEN 18082:2024) has been prepared by Technical Committee CEN/TC 275 “Food
analysis - Horizontal methods”, the secretariat of which is held by DIN.
This document is currently submitted to the CEN Enquiry.
WARNING — The use of this document can involve hazardous materials, operations and equipment. This
document does not purport to address all the safety problems associated with its use. It is the
responsibility of the user of this document to establish appropriate safety and health practices and
determine the applicability of regulatory limitations prior to use.
1 Scope
This document specifies a method for the analysis of pesticide residues in foods of animal origin with a
fat content of up to approximatively 10 %, such as meat, egg or milk by LC-MS/MS. Because of the low
material requirements for miniaturized processing and the few work steps, the process is particularly
time and cost-saving with high reliability and effectiveness. The method has been collaboratively studied
on a number of commodity/pesticide combinations. Precision data are summarized in Table B.1.
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 that 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, Foodstuffs — Guidelines for the calibration and quantitative determination of pesticide
residues and organic contaminants using chromatographic methods
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at https://www.electropedia.org/
4 Principle
Water is added to the homogeneous sample and is extracted with the help of acetonitrile. After addition
of magnesium sulfate, sodium chloride and buffering citrate salts, the mixture is shaken intensively and
centrifuged for phase separation. An aliquot of the organic phase is cleaned-up by dispersive solid phase
extraction (D-SPE) with amino-sorbents (e.g. primary secondary amine sorbent, PSA) as well as
magnesium sulfate for the removal of residual water. Following clean-up extracts are centrifuged. Fat
contained in the sample is removed by freezing out by storing the purified acetonitrile extract in the
freezer. The pesticides contained in the fat-free solution can be determined directly by LC-based analysis.
For the analysis with LC hyphenations with tandem mass-spectrometry (LC-MS/MS) or high resolution
mass-spectrometry (LC-HR-MS) are particularly suitable. Quantification may be performed using an
internal standard, which is added to the test portion before the first extraction, but this is not mandatory.
Details for calibration, see 7.2.
5 Preparation and storage of the samples
5.1 General
Sample processing and storage procedures should be demonstrated to have no significant effect on the
residues present in the test sample (sometimes also called “analytical sample”). Processing should also
ensure that the test sample is homogeneous enough so that portion to portion (sub-sampling) variability
is acceptable. If a single analytical portion is unlikely to be representative of the test sample, larger or
replicate portions shall be analysed, to provide a better estimate of the true value. The degree of
comminution should support a quantitative residue extraction. Otherwise, the extraction shall be car
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