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ISO 20122:2024(en)
ISO - Cover page
Foreword
Introduction
1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Reagents
6 Apparatus
7 Sample
 7.1 Sampling
 7.2 Preparation of the final sample for liquid and solid fats
8 Procedures
 8.1 General
 8.2 Hexane/ethanol distribution for removal of interfering substances
 8.3 Saponification
 8.4 Removal of biogenic n-alkanes with aluminium oxide for determination of the MOSH fraction
 8.5 Clean-up before epoxidation to separate polar substances
 8.6 Ethanolic epoxidation of the MOAH fraction to oxidize unsaturated non-aromatic compounds
 8.7 HPLC-GC separation
  8.7.1 HPLC conditions
  8.7.2 GC configuration
  8.7.3 Solvent vapour exit configuration
  8.7.4 Peak identification
  8.7.5 System suitability test
 8.8 Blank run
 8.9 Quality control
9 Result of the determination
 9.1 Testing the chromatograms for sufficient epoxidation and other relevant parameters
 9.2 Calculation
10 Precision of the method
 10.1 Repeatability limit
 10.2 Reproducibility limit
11 Test report
Annex A (informative) Graphics and chromatograms
Annex B (informative) Precision data
Annex C (informative) Alternative method for the epoxidation of the MOAH fraction (performic acid epoxidation)
Bibliography
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International

Standard

ISO 20122
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
Titre manque
Reference number
ISO 20122:2024(en)
First edition
2024-04
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ContentsPage

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 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).
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 at www.iso.org/members.html.

Introduction

In order to achieve a low limit of quantification (LOQ), the method contains additional and partially modified processing steps, specifications for the uniform processing of defined product groups and additional requirements for system suitability compared to EN 16995:2017.
The method has been tested in an interlaboratory study via the analysis of both naturally contaminated and spiked vegetable oil samples, ranging from 1 mg/kg to 75 mg/kg for MOSH, and from 1 mg/kg to 7 mg/kg for MOAH.
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International StandardISO 20122:2024(en)
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

1Scope

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).[4][5][6] 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).[14]

2Normative 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.
ISO 661, Animal and vegetable fats and oils — Preparation of test sample

3Terms and definitions

For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
ISO Online browsing platform: available at https://www.iso.org/obp
IEC Electropedia: available at https://www.electropedia.org/
3.1
mineral oil saturated hydrocarbons
MOSH
paraffinic (open-chain, usually branched) and naphthenic (cyclic, alkylated) hydrocarbons in the boiling range of n-alkanes with a chain length of 10 to 50 carbon atoms, which are obtained from mineral oil by this method by means of online-coupled high performance liquid chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID)
3.2
mineral oil aromatic hydrocarbons
MOAH
aromatic mainly alkylated hydrocarbons from mineral oil in the boiling range of n-alkanes with a chain length of 10 to 50 carbon atoms, determined by means of online-coupled high performance liquid chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID)
3.3
unresolved complex mixture
UCM
complex mixture of saturated or aromatic hydrocarbons not resolved by gas chromatography such as branched paraffins, alkylated naphthenes and alkylated aromatics, that produces a hump when analysed by gas chromatography-flame ionization detection (GC-FID)
3.4
polyolefin oligomeric saturated hydrocarbons
POSH
synthetic hydrocarbons from oligomers of polyolefins, such as polyethylene, polypropylene and polybutylenes
Note 1 to entry: Food contact uses comprise plastic bags, containers or films, heat sealable layers and other lamination as well as adhesives and plasticizers.
Note 2 to entry: POSH can be distinguished from mineral oil saturated hydrocarbons (MOSH) by their chromatographic pattern, but it is difficult to differentiate and chromatographically separate them from the MOSH if both are present.[5]
3.5
resin oligomeric saturated hydrocarbons
ROSH
synthetic saturated hydrocarbons (oligomers from monoterpenes, cyclopentadienes and other C5- or C9-monomeres) that are ingredients of hot-melt adhesives and can migrate into the sample mostly via gas phase transfer or via direct contact
3.6
resin oligomeric aromatic hydrocarbons
ROAH
synthetic aromatic hydrocarbons that are ingredients of hot-melt adhesives and can migrate into the sample mostly via gas phase transfer or by direct contact
3.7
poly-alpha-olefins
PAO
synthetic iso-paraffins with short and long side chains, used as lubricants or in adhesives and hotmelts
Note 1 to entry: When analysed by gas chromatography-flame ionization detection (GC-FID), they are recognized by series of rather narrow humps of unresolved branched hydrocarbons with regular distance between them.[5]
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Bibliography
[1]
ISO 5555, Animal and vegetable fats and oils — Sampling
[2]
ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results — Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method
[3]
EN 16995:2017, Foodstuffs — Vegetable oils and foodstuff on basis of vegetable oils — Determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) with on-line HPLC-GC-FID analysis
[4]
Biedermann, M., Fiselier, K., Grob, K. Aromatic hydrocarbons of mineral oil origin in foods: method for determining the total concentration and first results. J. Agric. Food Chem. 2009, 57 pp. 8711–8721
[5]
Biedermann, M., Grob, K. On-line coupled high performance liquid chromatography-gas chromatography (HPLC-GC) for the analysis of mineral oil: Part 1: method of analysis. J. Chromatogr. A. 2012, 1255 pp. 56–75
[6]
EFSA Panel on Contaminants in the Food Chain, Scientific Opinion on Mineral Oil Hydrocarbons in Food. EFSA Journal. 2012, 10(6) 2704
[7]
McGill, A., Moffat, C.F., Mackie, P.R., Cruickshank, P. The composition and concentration of n-alkanes in retail samples of edible oils. J. Sci. Food Agric. 1993, 61 pp. 357–362
[8]
Bratinova, S., Hoekstra, E. (eds) Guidance on sampling, analysis and data reporting for the monitoring of mineral oil hydrocarbons in food and food contact materials. JRC Technical Reports, 2019
[9]
Bundesinstitut für Risikobewertung, Berlin and Kantonales Labor Zürich. Measurement of Mineral Oil - Hydrocarbons in Food and Packaging Materials, 2012
[10]
Biedermann, M., Munoz, C., Grob, K. Update of on-line coupled liquid chromatography – gas chromatography for the analysis of mineral oil hydrocarbons in foods and cosmetics. J. Chromatrogr. A. 2017, 1521 pp. 140–149
[11]
Nestola, M., Schmidt, T.C. Determination of mineral oil aromatic hydrocarbons in edible oils and fats by online liquid chromatography-gas chromatography–flame ionization detection – Evaluation of automated removal strategies for biogenic olefins. J. Chromatogr. A. 2017, 1505 pp. 69–76, 2017
[12]
AOAC INTERNATIONAL. Definitions and calculations of Horrat values from intralaboratory data. Horrat for SLV.doc, 2004
[13]
Biedermann, M., Munoz, C., Grob, K. Epoxidation for the analysis of the mineral oil aromatic hydrocarbons in food. An update. J. Chromatogr. A. 2020, 1624 461236
[14]
Nestola, M. Automated workflow for the determination of mineral oil saturated and aromatic hydrocarbons (MOSH and MOAH) in edible oils and fats – Saponification and improved epoxidation as tools to increase sensitivity. J. Chromatogr. A. 2022, 1682 463523
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