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BS EN ISO 18363-2:2018

BS EN ISO 18363-2:2018

$142.49

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

Published By Publication Date Number of Pages
BSI 2018 32
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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.

PDF Catalog

PDF Pages PDF Title
2 National foreword
4 European foreword
7 Foreword
8 Introduction
11 1 Scope
2 Normative references
3 Terms and definitions
12 4 Principle
13 5 Reagents
5.1 General
5.2 Solvents and chemicals
5.2.1 Toluene.
5.2.3 Methanol.
5.2.5 Ethyl acetate.
5.2.6 Diethyl ether.
5.2.7 iso-Octane.
5.2.8 Sodium sulfate anhydrous, granular.
5.3 Standard and reference compounds
5.3.1 2-MCPD.
5.3.2 2-MCPD-d5.
5.3.3 2-MCPD-1,3-bis-stearoylester *.
5.3.4 2-MCPD-d5-1,3-bis-stearoylester *.
5.3.5 3-MCPD.
5.3.6 3-MCPD-d5.
5.3.7 3-MCPD-1,2-bis-palmitoylester *.
5.3.8 3-MCPD-d5-1,2-bis-palmitoylester *.
5.3.9 Glycidyl oleate*.
5.3.10 Glycidyl-d5 oleate*.
14 5.4 Working solutions**
5.4.2 2-MCPD-d5: 10,0 μg/ml in methanol.
5.4.3 3-MCPD: 10,0 μg/ml in methanol.
5.4.4 3-MCPD-d5: 10,0 μg/ml in methanol.
5.4.5 2-MCPD-1,3-bis-stearoyl ester: 29,1 μg/ml in toluene; equivalent to 5,0 μg/ml free 2-MCPD.
5.4.6 2-MCPD-d5-1,3-bis-stearoyl ester: 29,3 μg/ml in toluene; equivalent to 5,0 μg/ml free 2-MCPD.
5.4.7 3-MCPD-1,2-bis-palmitoyl ester: 26,6 μg/ml in toluene; equivalent to 5,0 μg/ml free 2-MCPD.
5.4.8 3-MCPD-d5-1,2-bis-palmitoyl ester: 26,8 μg/ml in toluene; equivalent to 5,0 μg/ml free 2-MCPD.
5.4.9 Glycidyl oleate: 22,8 μg/ml in toluene; equivalent to 5,0 μg/ml free glycidol.
5.4.10 Glycidyl-d5 oleate: 23,2 μg/ml in toluene; equivalent to 5,0 μg/ml free glycidol.
5.5 Other solutions
6 Apparatus
15 7 Sample
7.1 Sampling
7.2 Preparation of the test sample
8 Procedure
8.1 Spiking with surrogate standard and homogenization
8.2 Ester cleavage and glycidol transformation
16 8.3 Matrix removal
8.4 Derivatization
8.5 Gas chromatography/mass spectrometry references
17 9 Expression of results
9.1 Determination of bound glycidol
18 9.2 Determination of bound 2-MCPD
19 9.3 Determination of bound 3-MCPD
9.4 Determination of the degree of diester cleavage
20 9.5 Quality control
10 Notes
22 Annex A (informative) Examples of relevant chromatograms and data evaluation using “low-MCPD” palm oil
29 Annex B (informative) Results of interlaboratory tests
31 Bibliography

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BS EN ISO 18363-2:2018
$142.49