Vegetable oils - Determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) with online-coupled high performance liquid chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID) analysis - Method for low limit of quantification (ISO 20122:2024)

This document specifies a procedure for the determination of saturated and aromatic hydrocarbons (from C10 to C50) in vegetable fats and oils using the online-coupled high performance liquid chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID). This document does not apply to other matrices.
The method is applicable for the analysis of mineral oil saturated hydrocarbons (MOSH) and/or mineral oil aromatic hydrocarbons (MOAH).
According to the results of the interlaboratory studies, the method has been proven suitable for MOSH mass concentrations above 3 mg/kg and MOAH mass concentrations above 2 mg/kg.
In case of suspected interferences, the fossil origin of the MOSH and MOAH fraction can be verified by examination by GC⨯GC-MS.
An alternative method for the epoxidation of the MOAH fraction (performic acid epoxidation) is proposed in Annex C. This alternative method provides comparable results to the ethanolic epoxidation of the MOAH fraction described in 8.6. This alternative method for epoxidation has proven to be efficient for samples with a high amount of interferences in the MOAH fraction (e.g. tropical oils).

Pflanzliche Öle - Bestimmung von gesättigten Mineralölkohlenwasserstoffen (MOSH) und aromatischen Kohlenwasserstoffen (MOAH) mit Analyse durch online gekoppelte Hochleistungsflüssigkeitschromatographie-Gaschromatographie mit Flammenionisationsdetektion (HPLC‑GC‑FID) - Verfahren für die niedrige Bestimmungsgrenze (ISO 20122:2024)

Dieses Dokument legt ein Verfahren für die Bestimmung von gesättigten und aromatischen Kohlenwasserstoffen (von C10 bis C50) in pflanzlichen Fetten und Ölen mithilfe einer online gekoppelten Hochleistungsflüssigkeitschromatographie-Gaschromatographie mit Flammenionisationsdetektion (HPLC-GC-FID) fest [4] [5] [6]. Dieses Dokument ist nicht auf andere Matrizes anwendbar.
Das Verfahren ist anwendbar für die Analyse von gesättigten Mineralölkohlenwasserstoffen (MOSH, en: mineral oil saturated hydrocarbons) und/oder aromatischen Mineralölkohlenwasserstoffen (MOAH, en: mineral oil aromatic hydrocarbons).
Entsprechend den Ergebnissen des Ringversuchs hat sich das Verfahren für MOSH-Massenkonzentrationen über 3 mg/kg und für MOAH-Massenkonzentrationen über 2 mg/kg als geeignet erwiesen.
Bei Verdacht auf Störungen kann die fossile Herkunft der MOSH- und MOAH-Fraktion durch Untersuchung mit GC×GC-MS verifiziert werden.
In Anhang C wird ein alternatives Verfahren für die Epoxidierung der MOAH-Fraktion (Epoxidierung mit Per(oxy)ameisensäure) vorgeschlagen. Dieses alternative Verfahren liefert Ergebnisse, die mit denen der in 8.6 beschriebenen Ethanol-Epoxidierung der MOAH-Fraktion vergleichbar sind. Dieses alternative Verfahren für die Epoxidierung hat sich für Proben mit einem hohen Anteil an Störungen in der MOAH-Fraktion (z. B. tropische Öle) als leistungsfähig erwiesen [14].

Huiles végétales - Dosage des hydrocarbures saturés d’huile minérale (MOSH) et des hydrocarbures aromatiques d’huile minérale (MOAH) par analyse par chromatographie en phase liquide haute performance et chromatographie en phase gazeuse couplées à un détecteur à ionisation de flamme (CLHP-CG-FID) en ligne - Méthode pour une faible limite de quantification (ISO 20122:2024)

Le présent document spécifie un mode opératoire pour le dosage des hydrocarbures saturés et aromatiques (de C10 à C50) dans les matières grasses et huiles végétales en utilisant la chromatographie en phase liquide haute performance et la chromatographie en phase gazeuse couplées à un détecteur à ionisation de flamme (CLHP-CG-FID) en ligne. Le présent document ne s’applique pas à d’autres matrices.
La méthode s’applique à l’analyse des hydrocarbures saturés d’huile minérale (MOSH) et/ou des hydrocarbures aromatiques d’huile minérale (MOAH).
D’après les résultats des études interlaboratoires, il a été démontré que la méthode est adaptée pour des concentrations massiques de MOSH supérieures à 3 mg/kg et des concentrations massiques de MOAH supérieures à 2 mg/kg.
En cas de suspicion d’interférences, l’origine fossile des fractions MOSH et MOAH peut être vérifiée par un examen par chromatographie en phase gazeuse à deux dimensions, couplée à la spectrométrie de masse (CG⨯CG-SM).
Une méthode alternative d’époxydation de la fraction MOAH (époxydation par l’acide performique) est proposée dans l’Annexe C. Cette méthode donne des résultats comparables à l’époxydation éthanolique de la fraction MOAH décrite en 8.6. Cette méthode alternative d’époxydation s’est avérée efficace pour les échantillons présentant de fortes interférences dans la fraction MOAH (par exemple, les huiles tropicales).

Rastlinska olja - Določevanje nasičenih ogljikovodikov mineralnih olj (MOSH) in aromatskih ogljikovodikov mineralnih olj (MOAH) s spletno povezano tekočinsko kromatografijo visoke ločljivosti - plinsko kromatografijo - plamensko ionizacijsko detekcijo (HPLC-GC-FID) - Metoda za nizko mejo določljivosti (ISO 20122:2024)

SIST EN ISO 20122:2024

General Information

Status
Published
Publication Date
16-Apr-2024
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
17-Apr-2024
Due Date
24-Nov-2025
Completion Date
17-Apr-2024

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SLOVENSKI STANDARD
01-junij-2024
Rastlinska olja - Določevanje nasičenih ogljikovodikov mineralnih olj (MOAH) in
aromatskih ogljikovodikov mineralnih olj (MOAH) z on-line sklopljeno analizo s
tekočinsko kromatografijo visoke ločljivosti in plinsko kromatografijo v povezavi s
plamenskim ionizacijskim detektorjem (HPLC-GC-FID) - Metoda za nizko mejo
določljivosti (ISO 20122:2024)
Vegetable oils - Determination of mineral oil saturated hydrocarbons (MOSH) and
mineral oil aromatic hydrocarbons (MOAH) with online-coupled high performance liquid
chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID)
analysis - Method for low limit of quantification (ISO 20122:2024)
Pflanzliche Öle - Bestimmung von gesättigten Mineralölkohlenwasserstoffen (MOSH)
und aromatischen Kohlenwasserstoffen (MOAH) mit online gekoppelter HPLC-GC-FID-
Analyse - Verfahren für die niedrige Bestimmungsgrenze (ISO 20122:2024)
Huiles végétales - Dosage des hydrocarbures saturés d’huile minérale (MOSH) et des
hydrocarbures aromatiques d’huile minérale (MOAH) par analyse par chromatographie
en phase liquide haute performance et chromatographie en phase gazeuse couplées à
un détecteur à ionisation de flamme (CLHP-CG-FID) en ligne - Méthode pour une faible
limite de quantification (ISO 20122:2024)
Ta slovenski standard je istoveten z: EN ISO 20122:2024
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.

EN ISO 20122
EUROPEAN STANDARD
NORME EUROPÉENNE
April 2024
EUROPÄISCHE NORM
ICS 67.200.10
English Version
Vegetable oils - Determination of mineral oil saturated
hydrocarbons (MOSH) and mineral oil aromatic
hydrocarbons (MOAH) with online-coupled high
performance liquid chromatography-gas chromatography-
flame ionization detection (HPLC-GC-FID) analysis -
Method for low limit of quantification (ISO 20122:2024)
Huiles végétales - Dosage des hydrocarbures saturés Pflanzliche Öle - Bestimmung von gesättigten
d'huile minérale (MOSH) et des hydrocarbures Mineralölkohlenwasserstoffen (MOSH) und
aromatiques d'huile minérale (MOAH) par analyse par aromatischen Kohlenwasserstoffen (MOAH) mit online
chromatographie en phase liquide haute performance gekoppelter HPLC-GC-FID-Analyse - Verfahren für die
et chromatographie en phase gazeuse couplées à un niedrige Bestimmungsgrenze (ISO 20122:2024)
détecteur à ionisation de flamme (CLHP-CG-FID) en
ligne - Méthode pour une faible limite de quantification
(ISO 20122:2024)
This European Standard was approved by CEN on 12 January 2024.

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, 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, Türkiye 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
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 20122:2024 E
worldwide for CEN national Members.

Contents Page
European foreword . 3

European foreword
This document (EN ISO 20122:2024) 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 October 2024, and conflicting national standards shall
be withdrawn at the latest by October 2024.
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.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
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, 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, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 20122:2024 has been approved by CEN as EN ISO 20122:2024 without any modification.

International
Standard
ISO 20122
First edition
Vegetable oils — Determination of
2024-04
mineral oil saturated hydrocarbons
(MOSH) and mineral oil aromatic
hydrocarbons (MOAH) with
online-coupled high performance
liquid chromatography-gas
chromatography-flame ionization
detection (HPLC-GC-FID) analysis
— Method for low limit of
quantification
Reference number
ISO 20122:2024(en) © ISO 2024
ISO 20122:2024(en)
© ISO 2024
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
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
ISO 20122:2024(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
6 Apparatus . 6
7 Sample . 7
7.1 Sampling .7
7.2 Preparation of the final sample for liquid and solid fats .7
8 Procedures . 8
8.1 General .8
8.2 Hexane/ethanol distribution for removal of interfering substances .8
8.3 Saponification . .8
8.4 Removal of biogenic n-alkanes with aluminium oxide for determination of the MOSH
fraction .9
8.5 Clean-up before epoxidation to separate polar substances .9
8.6 Ethanolic epoxidation of the MOAH fraction to oxidize unsaturated non-aromatic
compounds .9
8.7 HPLC-GC separation .10
8.7.1 HPLC conditions .10
8.7.2 GC configuration .10
8.7.3 Solvent vapour exit configuration .11
8.7.4 Peak identification .11
8.7.5 System suitability test . 12
8.8 Blank run . 13
8.9 Quality control . 13
9 Result of the determination .13
9.1 Testing the chromatograms for sufficient epoxidation and other relevant parameters. 13
9.2 Calculation .14
10 Precision of the method .15
10.1 Repeatability limit . 15
10.2 Reproducibility limit . 15
11 Test report .15
Annex A (informative) Graphics and chromatograms.
...


SLOVENSKI STANDARD
01-junij-2024
Rastlinska olja - Določevanje nasičenih ogljikovodikov mineralnih olj (MOSH) in
aromatskih ogljikovodikov mineralnih olj (MOAH) s spletno povezano tekočinsko
kromatografijo visoke ločljivosti - plinsko kromatografijo - plamensko ionizacijsko
detekcijo (HPLC-GC-FID) - Metoda za nizko mejo določljivosti (ISO 20122:2024)
Vegetable oils - Determination of mineral oil saturated hydrocarbons (MOSH) and
mineral oil aromatic hydrocarbons (MOAH) with online-coupled high performance liquid
chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID)
analysis - Method for low limit of quantification (ISO 20122:2024)
Pflanzliche Öle - Bestimmung von gesättigten Mineralölkohlenwasserstoffen (MOSH)
und aromatischen Kohlenwasserstoffen (MOAH) mit online gekoppelter HPLC-GC-FID-
Analyse - Verfahren für die niedrige Bestimmungsgrenze (ISO 20122:2024)
Huiles végétales - Dosage des hydrocarbures saturés d’huile minérale (MOSH) et des
hydrocarbures aromatiques d’huile minérale (MOAH) par analyse par chromatographie
en phase liquide haute performance et chromatographie en phase gazeuse couplées à
un détecteur à ionisation de flamme (CLHP-CG-FID) en ligne - Méthode pour une faible
limite de quantification (ISO 20122:2024)
Ta slovenski standard je istoveten z: EN ISO 20122:2024
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.

EN ISO 20122
EUROPEAN STANDARD
NORME EUROPÉENNE
April 2024
EUROPÄISCHE NORM
ICS 67.200.10
English Version
Vegetable oils - Determination of mineral oil saturated
hydrocarbons (MOSH) and mineral oil aromatic
hydrocarbons (MOAH) with online-coupled high
performance liquid chromatography-gas chromatography-
flame ionization detection (HPLC-GC-FID) analysis -
Method for low limit of quantification (ISO 20122:2024)
Huiles végétales - Dosage des hydrocarbures saturés Pflanzliche Öle - Bestimmung von gesättigten
d'huile minérale (MOSH) et des hydrocarbures Mineralölkohlenwasserstoffen (MOSH) und
aromatiques d'huile minérale (MOAH) par analyse par aromatischen Kohlenwasserstoffen (MOAH) mit online
chromatographie en phase liquide haute performance gekoppelter HPLC-GC-FID-Analyse - Verfahren für die
et chromatographie en phase gazeuse couplées à un niedrige Bestimmungsgrenze (ISO 20122:2024)
détecteur à ionisation de flamme (CLHP-CG-FID) en
ligne - Méthode pour une faible limite de quantification
(ISO 20122:2024)
This European Standard was approved by CEN on 12 January 2024.

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, 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, Türkiye 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
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 20122:2024 E
worldwide for CEN national Members.

Contents Page
European foreword . 3

European foreword
This document (EN ISO 20122:2024) 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 October 2024, and conflicting national standards shall
be withdrawn at the latest by October 2024.
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.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
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, 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, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 20122:2024 has been approved by CEN as EN ISO 20122:2024 without any modification.

International
Standard
ISO 20122
First edition
Vegetable oils — Determination of
2024-04
mineral oil saturated hydrocarbons
(MOSH) and mineral oil aromatic
hydrocarbons (MOAH) with
online-coupled high performance
liquid chromatography-gas
chromatography-flame ionization
detection (HPLC-GC-FID) analysis
— Method for low limit of
quantification
Reference number
ISO 20122:2024(en) © ISO 2024
ISO 20122:2024(en)
© ISO 2024
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
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
ISO 20122:2024(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
6 Apparatus . 6
7 Sample . 7
7.1 Sampling .7
7.2 Preparation of the final sample for liquid and solid fats .7
8 Procedures . 8
8.1 General .8
8.2 Hexane/ethanol distribution for removal of interfering substances .8
8.3 Saponification . .8
8.4 Removal of biogenic n-alkanes with aluminium oxide for determination of the MOSH
fraction .9
8.5 Clean-up before epoxidation to separate polar substances .9
8.6 Ethanolic epoxidation of the MOAH fraction to oxidize unsaturated non-aromatic
compounds .9
8.7 HPLC-GC separation .10
8.7.1 HPLC conditions .10
8.7.2 GC configuration .10
8.7.3 Solvent vapour exit configuration .11
8.7.4 Peak identification .11
8.7.5 System suitability test . 12
8.8 Blank run . 13
8.9 Quality control . 13
9 Result of the determination .13
9.1 Testing the chromatograms for sufficient epoxidation and other relevant parameters. 13
9.2 Calculation .14
10 Precision of the method .15
10.1 Repeatability limit . 15
10.2 Reproducibility limit . 15
11 Test report .15
Annex A (informative) Graphics and chromatograms.
...

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