prEN 18032
(Main)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)
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 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 Meta boliten 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 wickelt[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/TS17061:2019 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 s kislim metanolom in merjenjem z LC- ali IC-MS/MS (QuPPe-Metoda)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-marec-2024
Živila - Hitra metoda za analizo več visokopolarnih pesticidov in njihovih
metabolitov v živilih z ekstrakcijo s kislim metanolom in merjenjem z LC- ali IC-
MS/MS (QuPPe-Metoda)
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: prEN 18032
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.
DRAFT
EUROPEAN STANDARD
NORME EUROPÉENNE
EUROPÄISCHE NORM
November 2023
ICS
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)
Lebensmittel ¿ Schnellmethode zur Bestimmung Produit alimentaire - Méthode rapide pour l'analyse de
mehrerer hochpolarer Pestizide und ihrer Metaboliten plusieurs pesticides hautement polaires et de leurs
in Lebensmitteln nach Extraktion mit angesäuertem métabolites dans les aliments impliquant une
Methanol und Messung mittels LC- oder IC-MS/MS extraction avec du méthanol acidifié et une mesure par
(QuPPe-Methode) LC- ou IC-MS/MS (QuPPe-Methode)
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
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 18032:2023 E
worldwide for CEN national Members.
prEN 18302:2023 (E)
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 . 4
5.1 General considerations . 4
5.2 Laboratory sample . 5
5.3 Treatment of laboratory samples prior to milling . 5
5.4 Sample homogenization . 5
5.4.1 General considerations . 5
5.4.2 Preparation of homogenates of dried fruit and similar commodities . 6
5.5 Analytical test portion . 6
6 Procedure . 7
7 Evaluation of results . 20
7.1 Identification . 20
7.2 Calibration and quantification . 20
7.3 Calculation of residue levels . 21
7.3.1 Calculation of residue concentrations using external calibration without IL-ISs. 21
7.3.2 Calculation of residue concentrations using external calibration and IL-IS . 22
7.3.3 Calculation of residue concentration using the standard additions approach . 23
7.3.4 Calculation of residue levels of complex residue definitions . 23
8 Validity of the method . 23
9 Test report . 28
10 Additional information on analysis . 28
10.1 Extraction Time . 28
10.2 Scaling . 28
Annex A (informative) Description of modules . 29
Annex B (normative) Additional information . 75
Annex C (informative) Overview of “Online Supplement” . 83
Bibliography . 84
prEN 18302:2023 (E)
European foreword
This document (prEN 18302:2023) has been prepared by Technical Committee CEN/TC275 “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.
prEN 18302:2023 (E)
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
3 Terms and Definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological 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 can affect
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 or 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.
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, larger or
prEN 18302:2023 (E)
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, extraction shall involve
supplementary comminution, e.g. through a homogenizing device (A.2.2) or grinding aids (e.g. metal balls
(A.2.3)).
5.2 Laboratory sample
A laboratory sample is the sample arriving to the laboratory for analysis and should ideally be sampled
according to international sampling protocols [4], [5]. A laboratory sample that is extensively spoiled or
degraded should normally not be analysed. Samples associated with a shelf life should normally be
analysed within their stated shelf life. If possible, process laboratory samples immediately after arrival and
in any event, before any significant physical or chemical changes have taken place. If a laboratory sample
cannot be processed without delay, it should be stored under appropriate conditions to keep it fresh and
to minimize deterioration.
If the laboratory sample is in a state that does not require milling prior to analysis (e.g. juices, milk, and
cereal flour), stir or shake the sample well and then withdraw the analytical test portions directly. Where
the homogeneity of the sample is, however, not sufficient or the extraction of residues is expected to be
significantly compromised due to the presence of larger particles, intensive comminution should be
performed using appropriate means.
5.3 Treatment of laboratory samples prior to milling
For preparation of the analytical sample, take only the portion of the laboratory sample to which the
maximum residue levels apply [6], [7].
...
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