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BS EN 17517:2021

$167.15

Animal feeding stuffs. Methods of sampling and analysis. Determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) with on-line HPLC-GC-FID analysis

Published By Publication Date Number of Pages
BSI 2021 44
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This document specifies a method for the determination of saturated and aromatic hydrocarbons (from C10 to C50) in feed. The method has been interlaboratory validated with on-line-HPLC-GC-FID – see [1], [2] and [3]. This method is not intended to be applied to other matrices.

The method can be used for the analysis of mineral oil saturated hydrocarbons (MOSH) and/or mineral oil aromatic hydrocarbons (MOAH).

The method is applicable for feed materials, in particular vegetable oils and other fat rich feed materials, compound feeds and pre-mixtures. It is not applicable to additives or deodistillates.

NOTE 1 The method was not designed for encapsulated matrices.

The method has been tested in an interlaboratory study via the analysis of both naturally contaminated and spiked samples (pre-mixture, soybean meal, sunflower seeds, chicken feed, pig feed, vegetable oil) ranging from 3 mg/kg to 286 mg/kg for MOSH and from 1 mg/kg to 16 mg/kg for MOAH.

According to the results of the interlaboratory study, the method has been proven suitable for MOSH and MOAH mass concentrations, each above 10 mg/kg. However, the method was not fully validated during the collaborative study for the premixture sample due to too low concentrations of MOSH and MOAH. The method was also not fully validated during the collaborative study for the sunflower seeds sample due to a too low concentration of MOAH.

NOTE 2 The conclusions regarding MOAH are based on 4 analyte / matrix combinations while the IUPAC protocol [4] expects this to be a minimum of 5.

In case of suspected interferences from natural sources, the fossil origin of the MOSH and MOAH fraction can be verified by examination of the pattern by GC-MS.

For the determination of MOSH and MOAH in edible fats and oils, another CEN standard is also available: EN 16995. For more information see [5].

Annex C proposes a manual alternative method to on-line HPLC-GC-FID analysis that can be used as a screening method for the determination of MOSH.

PDF Catalog

PDF Pages PDF Title
2 undefined
7 1 Scope
2 Normative references
3 Terms and definitions
8 4 Principle
5 Reagents
11 6 Apparatus
12 7 Sampling
8 Preparation of the test sample
9 Preparation of the analytical sample
9.1 Fat extraction from feed sample
13 9.2 Procedure for fats and fat extracts
9.3 Blank
14 10 Liquid chromatography and gas chromatography
10.1 Liquid chromatography setup
10.2 Working conditions for HPLC
15 10.3 HPLC-GC-interface
16 10.4 Gas chromatography setup
10.5 Working conditions for GC
17 10.6 Solvent vapor exit
10.7 Peak identification
10.8 Performance of the HPLC-GC system
18 10.9 Quantitative determination of hydrocarbons attributed to mineral oil origin
19 11 Precision
11.1 Interlaboratory test
11.2 Repeatability
11.3 Reproducibility
12 Test report
21 Annex A (informative)Examples of chromatograms
27 Annex B (informative)Precision data
30 Annex C (informative)Determination of saturated hydrocarbons of mineral oil – Manual alternative method to on-line HPLC-GC-FID analysis
C.1 General
C.2 Principle
C.3 Reagents
32 C.4 Apparatus
33 C.5 Sampling
C.6 Preparation of the test sample
C.7 Procedure
C.7.1 Fat extraction from feed sample
C.7.1.1 General
C.7.1.2 Fatty material extraction from animal feed (fat content lower than 15 %)
C.7.1.3 Fatty material extraction from oilseeds (fat content higher than 30 %)
34 C.7.1.4 Fatty material extraction from oilseeds (fat content between 15 % and 30 %)
C.7.1.5 Evaporation of the solvent
C.7.2 Chromatography column preparation
C.7.2.1 Preparation of AgNO3 impregnated silica gel
C.7.2.2 Column packing
35 C.7.3 Isolation of the hydrocarbon fraction from the fatty extract (or the oil sample)
C.7.3.1 Oil sample preparation
C.7.3.2 Elution of the hydrocarbon fraction
C.7.4 Gas Chromatography
C.7.4.1 Gas chromatography setup
C.7.4.2 Working conditions for gas chromatography analysis
36 C.7.4.3 Peak identification
C.7.4.4 Performance of the gas chromatography system
C.7.5 Procedural blank
37 C.7.6 Quantitative determination
40 C.8 Determination of hydrocarbons attributed to mineral origin
C.9 Precision data
BS EN 17517:2021
$167.15