prEN ISO 18363-3

Animal and vegetable fats and oils - Determination of fatty-acid-bound chloropropanediols (MCPDs) and glycidol by GC/MS - Part 3: Method using acid transesterification and measurement for 2-MCPD, 3-MCPD and glycidol (ISO/FDIS 18363-3:2024)

This document specifies a procedure for the simultaneous determination of 2-MCPD esters (bound 2-MCPD), 3‐MCPD esters (bound 3‐MCPD) and glycidyl esters (bound glycidol) in a single assay, based on acid catalysed ester cleavage and derivatization of cleaved (free) analytes with phenylboronic acid (PBA) prior to GC/MS analysis.
This document is applicable to solid and liquid fats and oils. For all three analytes the limit of quantification (LOQ) is 0,1 mg/kg and the limit of detection (LOD) is 0,03 mg/kg.

Tierische und pflanzliche Fette und Öle - Bestimmung von fettsäuregebundenem Chlorpropandiol (MCPD) und Glycidol mittels GC/MS - Teil 3: Verfahren mittels Säureumesterung und Messung für 2-MCPD, 3-MCPD und Glycidol (ISO/FDIS 18363-3:2024)

Dieses Dokument legt ein Verfahren für die gleichzeitige Bestimmung von 2 MCPD-Estern (gebundenem 2 MCPD), 3 MCPD-Estern (gebundenem 3 MCPD) und Glycidylestern (gebundenem Glycidol) in einer einzigen Prüfung fest, basierend auf einer vor der GC/MS-Analyse erfolgenden säurekatalysierten Esterspaltung und Derivatisierung der abgespaltenen (freien) Analyten mit Phenylboronsäure (en: phenylboronic acid, PBA).
Dieses Dokument ist auf feste und flüssige Fette und Öle anwendbar. Für alle drei Analyten liegt die Quantifizierungsgrenze (LOQ, en: limit of quantification) bei 0,1 mg/kg und die Nachweisgrenze (LOD, en: limit of detection) bei 0,03 mg/kg.

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 3: Méthode par transestérification acide et mesure du 2-MCPD, du 3-MCPD et du glycidol (ISO/FDIS 18363-3:2024)

Le présent document spécifie un mode opératoire permettant la détermination simultanée des esters de 2-MCPD (2-MCPD lié), des esters de 3-MCPD (3-MCPD lié) et des esters de glycidol (glycidol lié) en un seul essai, basé sur le clivage des esters par catalyse acide et la dérivatisation des analytes clivés (libres) à l’acide phénylboronique (PBA) avant analyse par CPG/SM.
Le présent document est applicable aux corps gras solides et liquides. Pour l’ensemble des trois analytes, la limite de quantification (LOQ) est de 0,1 mg/kg et la limite de détection (LOD) est de 0,03 mg/kg.

Živalske in rastlinske maščobe ter olja - Določevanje maščobnokislinsko vezanih kloropropandiolov (MCPD) in glicidola z GC/MS - 3. del: Metoda z uporabo kislinske transesterifikacije in meritev 2-MCPD, 3-MCPD in glicidola (ISO/FDIS 18363-3:2024)

General Information

• Status: Not Published
• Publication Date: 07-Oct-2025
• 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
• Current Stage: 6055 - CEN Ratification completed (DOR) - Publishing
• Start Date: 05-Jul-2024
• Completion Date: 05-Jul-2024
• Ref Project: oSIST prEN ISO 18363-3:2024 - Animal and vegetable fats and oils - Determination of fatty-acid-bound chloropropanediols (MCPDs) and glycidol by GC/MS - Part 3: Method using acid transesterification and measurement for 2-MCPD, 3-MCPD and glycidol (ISO/FDIS 18363-3:2024)

Relations

• Revises: EN ISO 18363-3:2021 - Animal and vegetable fats and oils - Determination of fatty-acid-bound chloropropanediols (MCPDs) and glycidol by GC/MS - Part 3: Method using acid transesterification and measurement for 2-MCPD, 3-MCPD and glycidol (ISO 18363-3:2017)
• Effective Date: 06-Dec-2023

Standards Content (Sample)

SLOVENSKI STANDARD
01-maj-2024
Živalske in rastlinske maščobe ter olja - Določevanje maščobnokislinsko vezanih
kloropropandiolov (MCPD) in glicidola z GC/MS - 3. del: Metoda z uporabo
kislinske transesterifikacije in meritev 2-MCPD, 3-MCPD in glicidola (ISO/FDIS
18363-3:2024)
Animal and vegetable fats and oils - Determination of fatty-acid-bound
chloropropanediols (MCPDs) and glycidol by GC/MS - Part 3: Method using acid
transesterification and measurement for 2-MCPD, 3-MCPD and glycidol (ISO/FDIS
18363-3:2024)
Tierische und pflanzliche Fette und Öle - Bestimmung von fettsäuregebundenem
Chlorpropandiol (MCPD) und Glycidol mittels GC/MS - Teil 3: Verfahren mittels
Säureumesterung und Messung für 2-MCPD, 3-MCPD und Glycidol (ISO/FDIS 18363-
3:2024)
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 3: Méthode par transestérification acide et mesure du 2-MCPD, du
3-MCPD et du glycidol (ISO/FDIS 18363-3:2024)
Ta slovenski standard je istoveten z: prEN ISO 18363-3
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 18363-3
ISO/TC 34/SC 11
Animal and vegetable fats and
Secretariat: BSI
oils — Determination of fatty-acid-
Voting begins on:
bound chloropropanediols (MCPDs)
2024-03-12
and glycidol by GC/MS —
Voting terminates on:
2024-06-04
Part 3:
Method using acid
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 3: Méthode par transestérification acide et mesure du
2-MCPD, du 3-MCPD et du 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 18363-3:2024(en) © ISO 2024

FINAL DRAFT
ISO/FDIS 18363-3:2024(en)
International
Standard
ISO/FDIS 18363-3
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 3:
Method using acid
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 3: Méthode par transestérification acide et mesure du
2-MCPD, du 3-MCPD et du 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.
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Published in Switzerland Reference number
ISO/FDIS 18363-3:2024(en) © ISO 2024

ii
ISO/FDIS 18363-3:2024(en)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents . 2
5.1 Standard and reference compounds .2
5.2 Standard solutions .3
5.2.1 General .3
5.2.2 Stock solutions (1 mg/ml) .3
5.2.3 Working solutions .3
5.3 Other reagents .4
5.4 Reagent solutions .4
6 Apparatus . 5
7 Sample . 5
7.1 Sampling .5
7.2 Preparation of the test sample .5
8 Procedure . 6
8.1 Test sample preparation .6
8.2 Preparation of the calibration curve .7
8.3 Gas chromatography/mass spectrometry references .7
9 Expression of results . 8
9.1 Quantification of 3-MCPD esters .8
9.2 Quantification of 2-MCPD esters .8
9.3 Quantification of glycidyl esters .9
10 Precision . 10
10.1 General .10
10.2 Repeatability .10
10.3 Between-day reproducibility . .10
11 Test report . 10
Annex A (informative) Construction of the calibration curves .11
Annex B (informative) Results of the interlaboratory test .15
Bibliography . 17

iii
ISO/FDIS 18363-3:2024(en)
Foreword
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bodies (ISO member bodies). The work of preparing International Standards is normally carried out through
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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 18363-3:2017), of which it constitutes a minor
revision. The ch
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