Foodstuff - Quick Method for the Analysis of Multiple Highly Polar Pesticides and their Metabolites in Foodstuff Involving Extraction with Acidified Methanol and Measurement by LC- or IC-MS/MS (QuPPe-Method)

This document specifies a procedure for the analysis of residues of highly polar pesticides and metabolites, which are not amenable to common multiresidue methods, in various food commodities of plant and animal origin, including fruits, vegetables, cereals, pulses, oily seeds, nuts, milk, liver and honey. The method was developed at the EURL-SRM hosted at CVUA Stuttgart [1], [2], [3] and has been collaboratively studied on a large number of commodity/pesticide combinations. Guidelines for calibration are outlined in CEN/TS 17061:2019.

Lebensmittel - Schnellmethode zur Bestimmung mehrerer hochpolarer Pestizide und ihrer Metaboliten in Lebensmitteln nach Extraktion mit angesäuertem Methanol und Messung mittels LC- oder IC-MS/MS (QuPPe-Methode)

Dieses Dokument legt ein Verfahren zur Bestimmung von Rückständen hochpolarer Pestizide und ihrer Metaboliten in verschiedenen Arten von Lebensmitteln pflanzlichen und tierischen Ursprungs, einschließlich Obst, Gemüse, Getreide, Hülsenfrüchte, Ölsaaten, Nüsse, Milch, Leber und Honig, fest, die mit üblichen Multiverfahren nicht untersucht werden können. Das Verfahren wurde in dem beim CVUA Stuttgart ansässigen EURL SRM entwickelt [1], [2], [3] und ist in Ringversuchen an einer großen Zahl von Lebensmittel-Pestizid-Kombinationen näher untersucht worden. Leitlinien für die Kalibrierung sind in CEN/TS 17061:2019 dargelegt.

Produits alimentaires - Méthode rapide pour l'analyse de plusieurs pesticides hautement polaires et de leurs métabolites dans les aliments impliquant une extraction avec du méthanol acidifié et une analyse par LC- ou CI-SM/SM (méthode QuPPe)

Le présent document spécifie un mode opératoire pour l'analyse des résidus de pesticides et de métabolites hautement polaires, qui ne se prêtent pas aux méthodes multirésidus courantes, dans de nombreux produits alimentaires d'origine végétale et animale, notamment les fruits, les légumes, les céréales, les légumineuses, les graines oléagineuses, les noix, le lait, le foie et le miel. La méthode a été élaborée par le laboratoire de référence de l'Union Européen selon des méthodes monorésidus (EURL SRM) au CVUA de Stuttgart [1], [2], [3] et a fait l'objet d'une étude collaborative sur un grand nombre de combinaisons de produits/pesticides. Les lignes directrices concernant l'étalonnage sont décrites dans la CEN/TS 17061:2019.

Živila - Hitra metoda za analizo več visokopolarnih pesticidov in njihovih metabolitov v živilih z ekstrakcijo z zakisanim metanolom in merjenjem z LC- ali IC-MS/MS (metoda QuPPe)

General Information

Status
Published
Publication Date
07-Oct-2025
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
08-Oct-2025
Due Date
26-Aug-2025
Completion Date
08-Oct-2025
Standard
EN 18032:2025
English language
88 pages
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Standards Content (Sample)


SLOVENSKI STANDARD
01-december-2025
Živila - Hitra metoda za analizo več visokopolarnih pesticidov in njihovih
metabolitov v živilih z ekstrakcijo z zakisanim metanolom in merjenjem z LC- ali IC-
MS/MS (metoda QuPPe)
Foodstuff - Quick Method for the Analysis of Multiple Highly Polar Pesticides and their
Metabolites in Foodstuff Involving Extraction with Acidified Methanol and Measurement
by LC- or IC-MS/MS (QuPPe-Method)
Lebensmittel - Schnellmethode zur Bestimmung mehrerer hochpolarer Pestizide und
ihrer Metaboliten in Lebensmitteln nach Extraktion mit angesäuertem Methanol und
Messung mittels LC- oder IC-MS/MS (QuPPe-Methode)
Produit alimentaire - Méthode rapide pour l'analyse de plusieurs pesticides hautement
polaires et de leurs métabolites dans les aliments impliquant une extraction avec du
méthanol acidifié et une mesure par LC- ou IC-MS/MS (QuPPe-Methode)
Ta slovenski standard je istoveten z: EN 18032:2025
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.

EN 18032
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2025
EUROPÄISCHE NORM
ICS 67.050
English Version
Foodstuff - Quick Method for the Analysis of Multiple
Highly Polar Pesticides and their Metabolites in Foodstuff
Involving Extraction with Acidified Methanol and
Measurement by LC- or IC-MS/MS (QuPPe-Method)
Produits alimentaires - Méthode rapide pour l'analyse Lebensmittel - Schnellmethode zur Bestimmung
de plusieurs pesticides hautement polaires et de leurs mehrerer hochpolarer Pestizide und ihrer Metaboliten
métabolites dans les aliments impliquant une in Lebensmitteln nach Extraktion mit angesäuertem
extraction avec du méthanol acidifié et une analyse par Methanol und Messung mittels LC- oder IC-MS/MS
LC- ou CI-SM/SM (méthode QuPPe) (QuPPe-Methode)
This European Standard was approved by CEN on 11 August 2025.

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 standards 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 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.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2025 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 18032:2025 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Preparation and storage of the samples . 5
5.1 General considerations . 5
5.2 Laboratory sample . 5
5.3 Treatment of laboratory samples prior to milling . 5
5.4 Sample homogenization . 6
5.5 Analytical test portion . 7
6 Procedure . 7
7 Evaluation of results . 18
7.1 Identification . 18
7.2 Calibration and quantification . 18
7.3 Calculation of residue levels . 19
8 Validity of the method . 22
9 Test report . 26
10 Additional information on analysis . 26
10.1 Extraction Time . 26
10.2 Scaling . 26
Annex A (informative) Description of modules . 27
A.1 Reagents . 27
A.2 Apparatuses and utensils . 33
A.3 Extraction (E) modules . 34
A.4 Clean-up (C) modules . 42
A.5 Dilution (DL) Modules . 44
A.6 Measurement (M) Modules . 45
A.7 Quantification (Q) Modules. 67
Annex B (normative) Additional information . 75
Annex C (informative) Supplementary information on the method . 84
Annex D (informative) Abbreviations and symbols . 85
Bibliography . 87

European foreword
This document (EN 18032:2025) has been prepared by Technical Committee CEN/TC275 “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 latest by April 2026, and conflicting national standards shall be withdrawn
at the latest by April 2026.
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.
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.
Any feedback and questions on this document should be directed to the users’ national standards body. A
complete listing of these bodies can be found on the CEN website.
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, 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 the United
Kingdom.
1 Scope
This document specifies a procedure for the analysis of residues of highly polar pesticides and metabolites,
which are not amenable to common multiresidue methods, in various food commodities of plant and
animal origin, including fruits, vegetables, cereals, pulses, oily seeds, nuts, milk, liver and honey. The
method was developed at the EURL-SRM hosted at CVUA Stuttgart [1], [2], [3] and has been collaboratively
studied on a large number of commodity/pesticide combinations. Guidelines for calibration are outlined
in CEN/TS 17061:2019.
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 17061:2019, Foodstuffs - Guidelines for the calibration and quantitative determination of pesticide
residues and organic contaminants using chromatographic methods
SANTE/11312/2021v2, Analytical quality control and method validation procedures for pesticide residues
analysis in food and feed
3 Terms and definitions
For the purposes of this document, the terms and definitions given in SANTE/11312/2021v2 apply.
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
Residues are extracted from the homogeneous test portion following water adjustment and addition of
acidified methanol. In the case of fruits and vegetables, the mixture is centrifuged, filtered and directly
analysed by LC-MS/MS or IC-MS/MS. In the case of cereals, pulses, nuts, oily seeds and foods of animal
origin, EDTA is added for the complexation of metal ions, such as calcium and magnesium, which positively
affects the analysis of certain compounds (e.g. glyphosate and AMPA). As such commodities also contain a
substantial content of protein, they are additionally diluted with acetonitrile to precipitate proteins.
Samples with high lipid content are subjected to dispersive SPE with C18-sorbent. Various LC- and IC-
MS/MS methods, allowing simultaneous analysis of different combinations of pesticides, are provided in
this document. Quantification is performed employing isotope-labelled analogues of the target analytes as
internal standards (IL-ISs), so far these are available. When adding IL-ISs directly to the test portion at the
beginning of the procedure, they compensate for any factors having an influence on recovery-rates, such
as volume-deviations and analyte losses during sample preparation. Matrix-effects during measurement
are also corrected. The use of IL-ISs, ensures good accuracy and reproducibility. Quantification without IL-
ISs is possible, but careful water adjustment and other approaches for addressing recovery losses and
matrix effects are required in this case. The analytical procedure entails few working steps and involves
little material consumption. A brief overview of the method is shown in the flowcharts within the “On-line
Supplement” linked in Annex C. Abbreviations and symbols are listed in Annex D.

Version 2 of 2021. Implemented as of 01/01/2024.
Available at: https://www.eurl-pesticides.eu/docs/public/tmplt_article.asp?CntID=727
5 Preparation and storage of the samples
5.1 General considerations
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 sub-sampling (portion-to-portion) variability
is acceptable. If a single analytical portion is unlikely to be representative of the test sample, lar
...

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