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)

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

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 (ISO/FDIS 18363-2:2024)

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 ter olja - Določanje maščobno-kislinsko vezanih kloropropandiolov (MCPD) in glicidola z GC/MS - 2. del: Metoda z uporabo počasne alkalne transesterifikacije in meritev 2-MCPD, 3-MCPD in glicidola (ISO/FDIS 18363-2:2024)

General Information

Status
Not Published
Public Enquiry End Date
30-Oct-2024
Current Stage
4020 - Public enquire (PE) (Adopted Project)
Start Date
05-Sep-2024
Due Date
23-Jan-2025
Completion Date
30-Oct-2024

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SLOVENSKI STANDARD
01-oktober-2024
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/FDIS 18363-2:2024)
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)
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
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 (ISO/FDIS 18363-2:2024)
Ta slovenski standard je istoveten z: prEN ISO 18363-2
ICS:
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.

FINAL DRAFT
International
Standard
ISO/FDIS 18363-2
ISO/TC 34/SC 11
Animal and vegetable fats and
Secretariat: BSI
oils — Determination of fatty-acid-
Voting begins on:
bound chloropropanediols (MCPDs)
2024-08-28
and glycidol by GC/MS —
Voting terminates on:
2024-11-20
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
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 SUPPOR TING DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
ISO/CEN PARALLEL PROCESSING LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
Reference number
ISO/FDIS 18363-2:2024(en) © ISO 2024

FINAL DRAFT
ISO/FDIS 18363-2:2024(en)
International
Standard
ISO/FDIS 18363-2
ISO/TC 34/SC 11
Animal and vegetable fats and
Secretariat: BSI
oils — Determination of fatty-acid-
Voting begins on:
bound chloropropanediols (MCPDs)
and glycidol by GC/MS —
Voting terminates on:
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
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 SUPPOR TING DOCUMENTATION.
© ISO 2024
IN ADDITION TO THEIR EVALUATION AS
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
ISO/CEN PARALLEL PROCESSING
LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
or ISO’s member body in the country of the requester.
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
ISO copyright office
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Email: copyright@iso.org
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Published in Switzerland Reference number
ISO/FDIS 18363-2:2024(en) © ISO 2024

ii
ISO/FDIS 18363-2:2024(en)
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 .9
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

iii
ISO/FDIS 18363-2:2024(en)
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,
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with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are described
in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the different types
of ISO document should be noted. This document was drafted in accordance with the editorial rules of the
ISO/IEC Directives, Part 2 (see www.iso.org/directives).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO had not received notice of (a)
patent(s) which may be required to implement this document. However, implementers are cautioned that
this may not represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and expressions
related to conformity assessment, as well as information about ISO’s adherence to the World Trade
Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11,
Animal and vegetable fats and oils, in collaboration with the European Committee for Standardization (CEN)
Technical Committee CEN/TC 307, Oilseeds, vegetable and animal fats and oils and their by-products - Methods
of sampling and analysis, in accordance with the Agreement on technical cooperation between ISO and CEN
(Vienna Agreement).
This second edition cancels and replaces the first edition (ISO 18363-2:2018), of which it constitutes a minor
revision to align the Introduction with ISO 18363-4:2021.
A list of all parts in the ISO 18363 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found a
...

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