EN ISO 18363-2:2018

Animal and vegetable fats and oils - Determination of fatty-acid-bound chloropropanediols (MCPDs) and glycidol by GC/MS - Part 2: Method using slow alkaline transesterification and measurement for 2-MCPD, 3-MCPD and glycidol (ISO 18363-2:2018)

This document specifies a procedure for the parallel determination of glycidol together with 2-MCPD and 3-MCPD present in bound or free form in oils and fats. The method is based on alkaline-catalysed ester cleavage, transformation of the released glycidol into monobromopropanediol (MBPD) and derivatisation of the derived free diols (MCPD and MBPD) with phenylboronic acid (PBA). Though free MCPD and glycidol are supposed to be present in fats and oils in low to negligible quantities only, in the event that free analytes are present, they would contribute proportionately to the results.  The results always being the sum of the free and the bound form of a single analyte.
This method is applicable to solid and liquid fats and oils. This document can also apply to animal fats and used frying oils and fats, but a validation study is undertaken before the analysis of these matrices.
Milk and milk products (or fat coming from milk and milk products) are excluded from the scope of this document.

Tierische und pflanzliche Fette und Öle - Bestimmung von fettsäuregebundenem Chlorpropandiol (MCPD) und Glycidol mittels GC/MS - Teil 2: Verfahren mittels langsamer alkalischer Umesterung und Messung für 2-MCPD, 3-MCPD und Glycidol (ISO 18363-2:2018)

Corps gras d'origines animale et végétale - Détermination des esters de chloropropanediols (MCPD) et d'acides gras et des esters de glycidol et d'acides gras par CPG/SM - Partie 2: Méthode par transestérification alcaline et mesure pour le 2-MCPD, le 3-MCPD et le glycidol (ISO 18363-2:2018)

Le présent document décrit un mode opératoire permettant la détermination parallèle du glycidol ainsi que du 2-MCPD et du 3-MCPD présents sous forme liée ou libre dans les corps gras. La méthode repose sur un clivage des esters par catalyse alcaline, une transformation du glycidol ainsi libéré en monobromopropanediol (MBPD) et une dérivatisation des diols libres (MCPD et MBPD) en présence d'acide phénylboronique (PBA). Même si les corps gras ne sont censés contenir que des quantités faibles voire négligeables de MCPD libre et de glycidol libre, une teneur importante augmenterait proportionnellement la détermination des analytes liés.
La présente méthode est applicable aux corps gras solides et liquides. Le présent document peut également s'appliquer aux graisses animales et aux huiles de friture usagées, mais une étude de validation est menée avant de procéder à l'analyse de ces matrices.
Le lait et les produits laitiers (ou les corps gras issus du lait et des produits laitiers) sont exclus du domaine d'application du présent document.

Živalske in rastlinske maščobe in olja - Ugotavljanje na maščobno kislino vezanih kloropropanediolov (MCPD) in glicidola z GC/MS - 2. del: Metoda z uporabo počasnega alkalnega preestrenja in meritev 2-MCPD, 3-MCPD in glicidola (ISO 18363-2:2018)

Ta del standarda ISO 18363 opisuje postopek za vzporedno ugotavljanje glicidola z 2-MCPD in 3-MCPD, prisotnega v vezanih ali prostih oljih in maščobah. Ta metoda temelji na alkalno katalizirani cepitvi estra, pretvarjanju sproščenega glicidola v monobromopropandiol (MBPD) in izpeljane proste diole (MCPD in MBPD) s fenilborovo kislino (PBA). Čeprav bi naj bila prosti MCPD in glicidol prisotna v maščobah ter oljih samo v nizkih do zanemarljivih količinah, bi velika vsebnost sorazmerno povečala ugotavljanje vezanih analitov.
Ta metoda se uporablja za trdne in tekoče maščobe ter olja. Ta del standarda ISO 18363 se lahko uporablja tudi za živalske maščobe ter uporabljena olja in maščobe za cvrtje, vendar je treba pred analizo teh matrik izvesti predhodno validacijsko študijo.
Mleko in mlečni izdelki (ali maščoba iz mleka in mlečnih izdelkov) niso zajeti v tem mednarodnem standardu.

General Information

• Status: Published
• Publication Date: 02-Oct-2018
• Withdrawal Date: 29-Apr-2019
• ICS: 67.200.10 - Animal and vegetable fats and oils
• Technical Committee: CEN/TC 307 - Oilseeds, vegetables and animal fats and oils and their by-products - Methods of sampling and analys
• Drafting Committee: CEN/TC 307 - Oilseeds, vegetables and animal fats and oils and their by-products - Methods of sampling and analys
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 03-Oct-2018
• Completion Date: 03-Oct-2018
• Ref Project: SIST EN ISO 18363-2:2018 - Animal and vegetable fats and oils - Determination of fatty-acid-bound chloropropanediols (MCPDs) and glycidol by GC/MS - Part 2: Method using slow alkaline transesterification and measurement for 2-MCPD, 3-MCPD and glycidol (ISO 18363-2:2018)

Relations

• Revised: prEN ISO 18363-2 - Animal and vegetable fats and oils - Determination of fatty-acid-bound chloropropanediols (MCPDs) and glycidol by GC/MS - Part 2: Method using slow alkaline transesterification and measurement for 2-MCPD, 3-MCPD and glycidol (ISO/FDIS 18363-2:2024)
• Effective Date: 28-Feb-2024

Standards Content (Sample)

SLOVENSKI STANDARD
01-december-2018
äLYDOVNHLQUDVWOLQVNHPDãþREHLQROMD8JRWDYOMDQMHQDPDãþREQRNLVOLQRYH]DQLK
NORURSURSDQHGLRORY0&3'LQJOLFLGROD]*&06GHO0HWRGD]XSRUDER
SRþDVQHJDDONDOQHJDSUHHVWUHQMDLQPHULWHY0&3'0&3'LQJOLFLGROD,62

Animal and vegetable fats and oils - Determination of fatty-acid-bound
chloropropanediols (MCPDs) and glycidol by GC/MS - Part 2: Method using slow alkaline
transesterification and measurement for 2-MCPD, 3-MCPD and glycidol (ISO 18363-
2:2018)
Tierische und pflanzliche Fette und Öle - Bestimmung von fettsäuregebundenem
Chlorpropandiol (MCPD) und Glycidol mittels GC/MS - Teil 2: Verfahren mittels
langsamer alkalischer Umesterung und Messung für 2-MCPD, 3-MCPD und Glycidol
(ISO 18363-2:2018)
Corps gras d'origines animale et végétale - Détermination des esters de
chloropropanediols (MCPD) et d'acides gras et des esters de glycidol et d'acides gras
par CPG/SM - Partie 2: Méthode par transestérification alcaline et mesure pour le 2-
MCPD, le 3-MCPD et le glycidol (ISO 18363-2:2018)
Ta slovenski standard je istoveten z: EN ISO 18363-2:2018
ICS:
67.200.10 5DVWOLQVNHLQåLYDOVNH Animal and vegetable fats
PDãþREHLQROMD and oils
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN ISO 18363-2
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2018
EUROPÄISCHE NORM
ICS 67.200.10
English Version
Animal and vegetable fats and oils - Determination of fatty-
acid-bound chloropropanediols (MCPDs) and glycidol by
GC/MS - Part 2: Method using slow alkaline
transesterification and measurement for 2-MCPD, 3-MCPD
and glycidol (ISO 18363-2:2018)
Corps gras d'origines animale et végétale - Tierische und pflanzliche Fette und Öle - Bestimmung
Détermination des esters de chloropropanediols von fettsäuregebundenem Chlorpropandiol (MCPD)
(MCPD) et d'acides gras et des esters de glycidol et und Glycidol mittels GC/MS - Teil 2: Verfahren mittels
d'acides gras par CPG/SM - Partie 2: Méthode par langsamer alkalischer Umesterung und Messung für 2-
transestérification alcaline et mesure pour le 2-MCPD, MCPD, 3-MCPD und Glycidol (ISO 18363-2:2018)
le 3-MCPD et le glycidol (ISO 18363-2:2018)
This European Standard was approved by CEN on 22 September 2018.

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 ISO 18363-2:2018 E
worldwide for CEN national Members.

Contents Page
European foreword . 3

European foreword
This document (EN ISO 18363-2:2018) has been prepared by Technical Committee ISO/TC 34 "Food
products" in collaboration with Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats
and oils and their by-products - Methods of sampling and analysis” the secretariat of which is held by
AFNOR.
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 2019, and conflicting national standards shall be
withdrawn at the latest by April 2019.
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.
According to the CEN-CENELEC Internal Regulations, the national standards organizations 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.
Endorsement notice
The text of ISO 18363-2:2018 has been approved by CEN as EN ISO 18363-2:2018 without any
modification.
INTERNATIONAL ISO
STANDARD 18363-2
First edition
2018-08
Animal and vegetable fats and oils —
Determination of fatty-acid-bound
chloropropanediols (MCPDs) and
glycidol by GC/MS —
Part 2:
Method using slow alkaline
transesterification and measurement
for 2-MCPD, 3-MCPD and glycidol
Corps gras d'origines animale et végétale — Détermination des
esters de chloropropanediols (MCPD) et d'acides gras et des esters de
glycidol et d'acides gras par CPG/SM —
Partie 2: Méthode par transestérification alcaline lente et mesure
pour le 2-MCPD, le 3-MCPD et le glycidol
Reference number
ISO 18363-2:2018(E)
©
ISO 2018
ISO 18363-2:2018(E)
© ISO 2018
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
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Published in Switzerland
ii © ISO 2018 – All rights reserved

ISO 18363-2:2018(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents . 3
5.1 General . 3
5.2 Solvents and chemicals . 3
5.3 Standard and reference compounds . 3
5.4 Working solutions** . 4
5.5 Other solutions . 4
6 Apparatus . 4
7 Sample . 5
7.1 Sampling . 5
7.2 Preparation of the test sample . 5
8 Procedure. 5
8.1 Spiking with surrogate standard and homogenization . 5
8.2 Ester cleavage and glycidol transformation . 5
8.3 Matrix removal . 6
8.4 Derivatization . 6
8.5 Gas chromatography/mass spectrometry references . 6
9 Expression of results . 7
9.1 Determination of bound glycidol . 7
9.2 Determination of bound 2-MCPD . 8
9.3 Determination of bound 3-MCPD . 9
9.4 Determination of the degree of diester cleavage . 9
9.5 Quality control .10
10 Notes .10
Annex A (informative) Examples of relevant chromatograms and data evaluation using
“low-MCPD” palm oil .12
Annex B (informative) Results of interlaboratory tests.19
Bibliography .21
ISO 18363-2:2018(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its f
...