EN 15662:2018
(Main)Foods of plant origin - Multimethod for the determination of pesticide residues using GC- and LC-based analysis following acetonitrile extraction/partitioning and clean-up by dispersive SPE - Modular QuEChERS-method
Foods of plant origin - Multimethod for the determination of pesticide residues using GC- and LC-based analysis following acetonitrile extraction/partitioning and clean-up by dispersive SPE - Modular QuEChERS-method
This European Standard stipulates a method for the analysis of pesticide residues in foods of plant origin, such as fruits (including dried fruits), vegetables, cereals and many processed products thereof by using GC, GC-MS(/MS), and/or LC-MS(/MS). The method has been collaboratively studied on a large number of commodity/pesticide combinations. Precision data are summarized in FprCEN/TR 17063. Guidelines for calibration are outlined in FprCEN/TS 17061.
Pflanzliche Lebensmittel - Multiverfahren zur Bestimmung von Pestizidrückständen mit GC und LC nach Acetonitril-Extraktion/Verteilung und Reinigung mit dispersiver SPE - Modulares QuEChERS-Verfahren
Diese Europäische Norm beschreibt ein Verfahren für die Analyse von Pestizidrückständen in pflanzlichen Lebensmitteln wie z. B. Früchten (einschließlich Trockenfrüchten), Gemüse (einschließlich getrocknetem Gemüse), Getreide und vielen verarbeiteten Erzeugnissen aus diesen Produkten unter Verwendung von GC, GC MS(/MS) und/oder LC MS(/MS). Das Verfahren wurde im Ringversuch mit einer großen Anzahl an Rohstoff /Pestizidkombinationen geprüft. Die Präzisionsdaten sind in CEN/TR 17063 zusammen¬gefasst. Leitfäden für die Kalibrierung sind in CEN/TS 17061 angegeben.
Aliments d'origine végétale - Multiméthode de détermination des résidus de pesticides par analyse CG et CL après extraction/partition avec de l'acétonitrile et purification par SPE dispersive - Méthode modulaire QuEChERS
La présente Norme européenne décrit une méthode d’analyse CG, CG-SM(/SM) et/ou CL-SM(/SM) des résidus de pesticides dans les aliments d’origine végétale, notamment les fruits (y compris les fruits secs), les légumes (y compris les légumes secs), les céréales et les nombreux produits transformés dérivés de ceux-ci. La méthode a fait l’objet d’un essai interlaboratoires portant sur un grand nombre de combinaisons denrée/pesticide. Les données de fidélité sont résumées dans le CEN/TR 17063. Les lignes directrices relatives à l’étalonnage sont données dans le CEN/TS 17061.
Hrana rastlinskega izvora - Večelementna metoda za določanje ostankov pesticidov z uporabo analize na osnovi GC in LC po delitvi in izpiranju acetonitrila z disperzivno SPE - Modularna metoda QuEChERS
Ta evropski standard določa metodo za analizo ostankov pesticidov v živilih rastlinskega izvora, kot so sadje (vključno s suhim sadjem), zelenjava, žitarice in številni predelani izdelki rastlinskega izvora z uporabo GC, GC-MS(/MS) in/ali LC-MS(/MS). Ta metoda je bila raziskana z večstranskimi študijami na veliki količini kombinacij proizvodov in pesticidov. Podatki o natančnosti so povzeti v standardu FprCEN/TR 17063. Smernice za umerjanje so opisane v standardu FprCEN/TS 17061.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-julij-2018
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SIST EN 15662:2009
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Foods of plant origin - Multimethod for the determination of pesticide residues using GC-
and LC-based analysis following acetonitrile extraction/partitioning and clean-up by
dispersive SPE - Modular QuEChERS-method
Pflanzliche Lebensmittel - Multiverfahren zur Bestimmung von Pestizidrückständen mit
GC und LC nach Acetonitril-Extraktion/Verteilung und Reinigung mit dispersiver SPE -
Modulares QuEChERS-Verfahren
Aliments d'origine végétale - Multiméthode de détermination des résidus de pesticides
par analyse CG et CL après extraction/partition avec de l'acétonitrile et purification par
SPE dispersive - Méthode modulaire QuEChERS
Ta slovenski standard je istoveten z: EN 15662:2018
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 15662
EUROPEAN STANDARD
NORME EUROPÉENNE
May 2018
EUROPÄISCHE NORM
ICS 67.050 Supersedes EN 15662:2008
English Version
Foods of plant origin - Multimethod for the determination
of pesticide residues using GC- and LC-based analysis
following acetonitrile extraction/partitioning and clean-up
by dispersive SPE - Modular QuEChERS-method
Aliments d'origine végétale - Multiméthode de Pflanzliche Lebensmittel - Multiverfahren zur
détermination des résidus de pesticides par analyse CG Bestimmung von Pestizidrückständen mit GC und LC
et CL après extraction/partition avec de l'acétonitrile nach Acetonitril-Extraktion/Verteilung und Reinigung
et purification par SPE dispersive - Méthode modulaire mit dispersiver SPE - Modulares QuEChERS-Verfahren
QuEChERS
This European Standard was approved by CEN on 27 December 2017.
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, 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: Rue de la Science 23, B-1040 Brussels
© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 15662:2018 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Principle . 4
4 Preparation and storage of the samples . 4
5 Procedure. 5
6 Evaluation of results . 15
7 Confirmatory tests . 22
8 Precision . 22
9 Test report . 22
Annex A (informative) Description of modules . 23
Annex B (informative) Complementary information . 76
Annex C (informative) Abbreviations . 78
Bibliography . 80
European foreword
This document (EN 15662:2018) has been prepared by Technical Committee CEN/TC 275 “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 November 2018, and conflicting national standards
shall be withdrawn at the latest by November 2018.
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.
This document supersedes EN 15662:2008.
With the revised version, some amendments and improvements have been taken into consideration,
notably:
— the more precise differentiation between feasible modes of operation (Table 1 to Table 5);
— the opportunity to report the applied modes of operation (e.g. extraction or clean-up modules) in a
simple way;
— clear indications of approved modes of operation for particular commodities (Table 6);
— the optimization of extraction efficiency by longer extraction time;
— the specification of suitable parameters for the detection with UPLC-MS/MS and GC-MS/MS;
— new approaches for the quantitation of pesticide residues including a simplified procedure for the
calculation of residue levels;
— references to the improved validation data for the method (see Table 7 and CEN/TR 17063);
— a list of abbreviations has been added in Annex C.
WARNING — The application of this standard may involve hazardous materials, operations and
equipment. This standard does not claim to address all the safety problems associated with its
use. It is the responsibility of the user of this standard to establish appropriate safety and health
practices and to determine the applicability of regulatory limitations prior to use.
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, 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 the United Kingdom.
1 Scope
This European Standard stipulates a method for the analysis of pesticide residues in foods of plant
origin, such as fruits (including dried fruits), vegetables (including dried vegetables), cereals and many
processed products thereof by using GC, GC-MS(/MS), and/or LC-MS(/MS). The method has been
collaboratively studied on a large number of commodity/pesticide combinations. Precision data are
summarized in CEN/TR 17063. 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 17061:2017, Foodstuffs - Guidelines for the calibration and quantitative determination of
pesticide residues and organic contaminants using chromatographic methods
3 Principle
The homogeneous sample is extracted with the help of acetonitrile. Samples with low water content
(<80 %) require the addition of water before the initial extraction to get a total of approximately 10 g of
water. 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) employing bulk sorbents as well as magnesium sulfate for
the removal of residual water. Following clean-up with amino-sorbents (e.g. primary secondary amine
sorbent, PSA) and if necessary graphitized carbon black (GCB) or octadecylsilane (ODS), extracts are
acidified by adding a small amount of formic acid, to improve the storage stability of certain base-
sensitive pesticides. The final extract can be directly employed for GC- and LC-based analysis. Suitable
detectors for GC analysis are mass-selective detectors (MS or MS/MS) with unit or high mass resolution
or other GC detectors, such as flame photometric detector, FPD, and electron capture detector, ECD. For
the analysis with LC hyphenations with tandem mass-spectrometry (LC-MS/MS) or high resolution
mass-spectrometry 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 CEN/TS 17061.
4 Preparation and storage of the samples
4.1 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.
4.2 Laboratory sample
A laboratory sample that is wholly or extensively spoiled or degraded should not be analysed. When
possible, prepare 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 prepared without
delay, it should be stored under appropriate conditions to keep it fresh and to avoid deterioration.
Dried or similarly processed samples should be analysed within their stated shelf life.
4.3 Partly-prepared test sample
For preparation of the partly-prepared test sample take only the portion of the laboratory sample to
which the maximum residue level applies. No further plant-parts shall be removed.
The reduction of the laboratory sample shall be carried out in such a way that representative portions
are obtained (e.g. by sub-division into four and selection of opposite quarters). For samples of small
units (e.g. small fruits such as berries, legumes, cereals), the sample shall be thoroughly mixed before
weighing out the partly-prepared test sample. When the samples are made up of larger units, take
wedge-shaped sections (e.g. melons) or cross sections (e.g. cucumbers) that include the skin (outer
surface) from each unit [1].
4.4 Test sample
From each partly-prepared test sample, any parts that would cause difficulties with the homogenization
process should be removed. In the case of stone fruits, the stones shall be removed. This is the test
sample. A record of the plant-parts that have been removed shall be kept. Precautions should be taken
to avoid any losses of juice or flesh. Calculation of the residue shall be based on the mass of the original
test sample (including the stones where it is necessary).
Where the homogeneity of the test sample is not sufficient or the extraction of residues may be
significantly compromised due to large particle sizes, intensive comminution should be performed
using appropriate means. This is possible at ambient temperature, if separation of flesh and juice or
degradation of target pesticides does not occur to a significant extent. Comminution of samples in a
frozen state can significantly reduce losses of chemically labile pesticides and usually results in smaller
particle sizes and a higher degree of homogeneity. Cutting the samples coarsely (e.g. 3 cm x 3 cm) with a
knife and putting them into the freezer (e.g. −18 °C overnight) prior to comminution facilitates
processing. Processing can be also assisted and improved by cryogenic milling (using dry ice or liquid
nitrogen) by keeping the temperature below 0 °C. Especially in the case of fruits and vegetables,
cryogenic milling is much more effective at homogenizing commodities that have tough skins (e.g.
tomatoes or grapes) compared to milling at ambient temperature. Given the fact that non-systemic
pesticides often predominantly occur on the skin, cryogenic milling significantly reduces sub-sampling
variability. When processing test samples at low temperatures, condensation caused by hi
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