CEN/TS 17062:2019

Foods of plant origin - Multimethod for the determination of pesticide residues in vegetable oils by LC-MS/MS (QuOil)

This Technical Specification describes a method for the analysis of pesticide residues in fatty oils of plant origin (essential oils are excluded). It has been validated in an interlaboratory test with olive oil. However, laboratory experiences have shown that this method is also applicable to other kinds of oils such as sunflower seed oil, sesame oil, flax seed oil, rape seed oil, grape seed oil, thistle oil and pumpkin seed oil.

Pflanzliche Lebensmittel - Multiverfahren zur Bestimmung von Pestizidrückständen in pflanzlichen Ölen mit LC-MS/MS (QuOil)

Diese Technische Spezifikation beschreibt ein Verfahren zur Bestimmung von Pflanzenschutzmittel-rückständen in fettigen pflanzlichen Ölen (ätherische Öle werden nicht berücksichtigt). Das Verfahren wurde in einem Ringversuch mit Olivenöl validiert. Laborerfahrungen haben jedoch gezeigt, dass dieses Verfahren auch bei anderen Ölsorten wie Sonnenblumenkernöl, Sesamöl, Leinöl, Rapsöl, Traubenkernöl, Distelöl und Kürbiskernöl anwendbar ist.

Aliments d’origine végétale - Multiméthode de détermination des résidus de pesticides dans les huiles végétales par CL-SM/SM (QuOil)

La présente Spécification technique décrit une méthode d’analyse des résidus de pesticides dans les huiles grasses d’origine végétale (les huiles essentielles sont exclues). Elle a été validée lors d’un essai interlaboratoires avec de l’huile d’olive. Toutefois, les expériences menées en laboratoire montrent que cette méthode est également applicable à d’autres types d’huiles, telles que l’huile de tournesol, l’huile de sésame, l’huile de lin, l’huile de colza, l’huile de pépins de raisin, l’huile de chardon et l’huile de pépins de courge.

Hrana rastlinskega izvora - Multirezidualna metoda za določanje ostankov pesticidov v rastlinskih oljih z LC-MS/MS (QuOil)

Ta tehnična specifikacija opisuje metodo za analizo ostankov pesticidov v maščobnih oljih rastlinskega izvora (eterična olja niso zajeta). Potrjena je bila v okviru medlaboratorijskega preskusa z olivnim oljem. Rezultati laboratorijskih preskusov pa so pokazali, da se lahko ta metoda uporablja tudi za druge vrste olj, kot so olje iz sončničnih semen, sezamovo olje, olje iz lanenih semen, olje iz oljne repice, olje grozdnih pečk, olje iz semen žafranike in bučno olje.

General Information

• Status: Published
• Publication Date: 03-Sep-2019
• 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
• 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-TS CEN/TS 17062:2019 - Foods of plant origin - Multimethod for the determination of pesticide residues in vegetable oils by LC-MS/MS (QuOil)

Relations

• Replaces: CEN/TS 17062:2017 - Foods of plant origin - Multimethod for the determination of pesticide residues in vegetable oils by LC-MS/MS
• Effective Date: 11-Sep-2019

Standards Content (Sample)

SLOVENSKI STANDARD
01-november-2019
Nadomešča:
SIST-TS CEN/TS 17062:2017
Hrana rastlinskega izvora - Multirezidualna metoda za določanje ostankov
pesticidov v rastlinskih oljih z LC-MS/MS (QuOil)
Foods of plant origin - Multimethod for the determination of pesticide residues in
vegetable oils by LC-MS/MS (QuOil)
Pflanzliche Lebensmittel - Multiverfahren zur Bestimmung von Pestizidrückständen in
pflanzlichen Ölen mit LC-MS/MS (QuOil)
Aliments d’origine végétale - Multiméthode de détermination des résidus de pesticides
dans les huiles végétales par CL-SM/SM (QuOil)
Ta slovenski standard je istoveten z: CEN/TS 17062:2019
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
67.200.10 Rastlinske in živalske Animal and vegetable fats
maščobe in olja and oils
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

CEN/TS 17062
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
September 2019
TECHNISCHE SPEZIFIKATION
ICS 67.050
English Version
Foods of plant origin - Multimethod for the determination
of pesticide residues in vegetable oils by LC-MS/MS
(QuOil)
Aliments d'origine végétale - Multiméthode de Pflanzliche Lebensmittel - Multiverfahren zur
détermination des résidus de pesticides dans les huiles Bestimmung von Pestizidrückständen in pflanzlichen
végétales par CL-SM/SM (QuOil) Ölen mit LC-MS/MS (QuOil)
This Technical Specification (CEN/TS) was approved by CEN on 14 July 2019 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to
submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS
available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in
parallel to the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached.

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, 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
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17062:2019 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 Reagents . 4
6 Apparatus . 7
7 Procedure. 8
7.1 Extraction . 8
7.2 Clean-up . 8
7.3 Determination by liquid chromatography with tandem mass spectrometry (LC-
MS/MS) . 9
8 Evaluation of results . 9
8.1 Identification and quantification . 9
8.2 Calculation of residue concentrations using the internal standard . 10
8.3 Calculation of residue concentrations without internal standards . 10
8.4 Calculation of residue concentration using the standard additions approach . 10
9 Precision . 10
10 Test report . 11
Annex A (informative) Examples of experimental conditions . 12
Annex B (informative) Precision data and recovery . 15
Annex C (informative) Scheme of procedure (for 2 g of sample) . 24
Annex D (informative) Recovery studies . 25
Annex E (informative) Abbreviations . 26
Bibliography . 28

European foreword
This document (CEN/TS 17062:2019) 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.
This document will supersede CEN/TS 17062:2017.
Compared to CEN/TS 17062:2017, the following changes have been made:
— Annex E (informative) containing a list of abbreviations was added;
— The document has been editorially revised.
— Annex E (informative) contains a list of abbreviations.
WARNING — The application of this Technical Specification may involve hazardous materials,
operations and equipment. This Technical Specification does not claim to address all the safety
problems associated with its use. It is the responsibility of the user of this Technical
Specification 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 announce this Technical Specification: 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, Turkey and the
United Kingdom.
1 Scope
This Technical Specification describes a method for the analysis of pesticide residues in fatty oils of
plant origin (essential oils are excluded). It has been validated in an interlaboratory test with olive oil.
However, laboratory experiences have shown that this method is also applicable to other kinds of oils
such as sunflower seed oil, sesame oil, flax seed oil, rape seed oil, grape seed oil, thistle oil and pumpkin
seed oil.
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 — Guideline for the calibration and quantitative determination of
chromatographic methods for the determination of pesticide residues and organic contaminants
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:
• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at https://www.iso.org/obp
4 Principle
The homogeneous sample is extracted with acetonitrile. After centrifugation, an aliquot of the organic
phase is cleaned-up by dispersive solid phase extraction (D-SPE; sorbents PSA and C18). To separate
co-extracted fat a freeze-out step of the acetonitrile phase can be applied. After clean up an additional
centrifugation step is performed. The 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 used
for LC-MS/MS analysis. A scheme of the procedure is given in Annex C.
NOTE In contrast to the method described in EN 15662 [1], this procedure does not include any addition of
water.
5 Reagents
Unless otherwise specified, use reagents of recognized analytical grade. Take every precaution to avoid
possible contamination of water, solvents, sorbents, inorganic salts, etc.
5.1 Water, HPLC quality.
5.2 Acetonitrile, HPLC quality.
5.3 Methanol, HPLC quality.
5.4 Acetic acid.
5.5 Ammonium formate.
5.6 Formic acid solution in acetonitrile, volume concentration σ = 5 ml formic acid/100 ml :
Dilute 5 ml of formic acid (mass fraction w ≥ 95 %) to 100 ml with acetonitrile (5.2).
® 1)
5.7 Primary secondary amin sorbent (PSA), e.g. Bondesil-PSA 40 µm Agilent No. 12213023 .
Other amino sorbents may be used, but investigations may be necessary to prove equivalency especially
regarding analyte losses and pH value of the end extracts.
5.8 C-18-sorbent (Octadecyl-silyl-modified silica gel), Bulk material 50 µm.
5.9 Internal standard and quality control standard solutions in acetonitrile, mass concentration
ρ = 10 µg/ml to 100 µg/ml.
Table 1 shows a list of potential internal standards (ISTDs) and quality control (QC) standards that may
be used in this method.
Table 1 — Potential internal standards (ISTDs) or quality control (QC) standards
Compound Log P Suggested MS/MS MS/MS
(octanol-water concentration ESI (+) ESI (-)
partition C
ISTD
coefficient)
[µg/ml]
Tris-(1,3-dichlorisopropyl)- 3,65 10 +++ +
phosphate
Linuron-D6 3,00 10 ++ -
Carbofuran-D3 1,80 10 ++ -
Chlorpyrifos-D10 4,70 10 +++ -
Bis-nitrophenyl urea 3,76 10 - +++
(Nicarbazin)
+++ very good detectable
++ good detectable
+ poor detectable
- not detectable
5.10 Primary pesticide standards
Use standards of known purity, only.

1) ®
Bondesil-PSA is a product supplied by Agilent. This information is given for the convenience of users of this
European Technical Specification and does not constitute an endorsement by CEN of the product named.
Equivalent products may be used if they can be shown to lead to the same results.
5.11 Pesticide stock solutions
Prepare individual stock solutions of analytical standards at concentrations that are sufficient to allow
the preparation of complex pesticide working solutions that are used for the preparation of standard
solutions.
Usually, store stock solutions at ≤ −18 °C. Check the stability of stock solutions during storage regularly
[2]. In some cases the addition of acids or bases can be helpful to enhance stability and extend the
acceptable storage period. Before withdrawing any aliquot from this solution redissolve any
precipitation that may have occurred.
5.12 Pesticide working solutions
Because of the broad applicability of this method and due to the partly divergent pH-stability of
pesticides, more than one working solution each containing one or more pesticides can be needed to
cover the entire pesticide spectrum of interest. These are prepared by mixing together defined volumes
of the required pesticide stock solutions (5.11) and appropriately diluting them with acetonitrile. The
pesticide concentrations in these mixtures should be sufficient to allow the preparation of the required
matrix matched standards (5.13.2) with moderate dilution of the blank sample extract (e.g. less than
20 %).
Usually, pesticide working solutions should be stored at low temperature in the dark. Check the stability
of pesticides contained in these mixtures during storage regularly [2] and adapt the storing conditions
accordingly. In some cases the addition of acids or bases can be helpful to enhance stability and extend
acceptable storage times.
5.13 Standard solutions (calibration mixtures)
5.13.1 Solvent-based standards
Prepare solvent-based standards by mixing known volumes of the pesticide working solutions (5.12)
and make
...