Validation européenne de la détermination des hydrocarbures saturés (MOSH) et des hydrocarbures aromatiques (MOAH) d’huile minérale dans l’alimentation des animaux (CEN / TC327 / WG1)
Analyse, Lipides, Sécurité, Contaminants
Poster de Florence Lacoste, Responsable Département Analyse & Expertise, au 17ème Congrès Euro Fed Lipid, 20 octobre 2019 : « European validation of the determination of Mineral Oil Saturated Hydrocarbons (MOSH) and Mineral Oil Aromatic Hydrocarbons (MOAH) in animal feed (CEN/TC327/WG1) »
The Mandate M/523 for standardization was addressed by the European Commission to CEN in 2013, in order to provide standardized methods for the analysis of animal feed in the framework of the Regulation (EC 882/2004) on official controls performed to ensure the verification of compliance with feed and food law, animal health and animal welfare rules. Among the methods of analysis to be mandated, one of them was focused on the determination of mineral oils in additives, premixtures, feed materials, in particular vegetable oils and other fat rich feed materials, and compound feed.
An interlaboratory study was conducted in 2018 to evaluate a method for determining mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in animal feed, within CEN/TC327/WG1 workprogam.
The fatty material is extracted from the commodity using organic solvent. After concentration of part of the solvent, the extract is submitted to an epoxidation step. The fractions of MOSH and MOAH are isolated and separated by an HPLC-GC-FID system. MOSH and MOAH fractions are separated on a silica gel column using a hexane-dichloromethane gradient and each one are transferred to GC while triglycerides are kept on the HPLC column. MOSH and MOAH are quantitated by internal standard added before analysis. Verification standards are added monitoring proper HPLC fractionation and GC transfer conditions.
A set of 3 oil samples and 8 feed samples delivered in double blind were assayed by 10 collaborating laboratories from five European countries. Sample matrices included refined sunflower oil, crude soybean oil, bleached palm oil, sunflower seeds, soybean meal, premix, chicken feed, pig feed ranging from 3 mg/kg to 286 mg/kg for MOSH, and from 0.3 mg/kg to 16 mg/kg for MOAH. Reproducibility (RSDR) ranged from 11.1 % to 25.3 % for samples containing more than 10 mg/kg of MOSH. Reproducibility (RSDR) ranged from 8.6 % to 25.9 % for samples containing more than 10 mg/kg of MOAH. Based on the precision data, the limit of application of the method was fixed at 10 mg/kg for both MOSH and MOAH with the method as described.
The author would like to thank the following collaborators for their participation: Hugues Griffon, ITERG, France. Ludger Brühl, Max Rubner-Institut (MRI), Germany. Monika Mainka, SGS Institut Fresenius GmbH, Germany. Eileen Schulz, Institut Kirchhoff Berlin GmbH, Germany. Thomas Funke, Mas GmbH, Germany. Christophe Goldbeck, Chemisches und Veterinäruntersuchungsamt Münsterland-Emscher-Lippe (CVUA-MEL), Germany. Sabrina Moret, University of Udine, Italy. Emiliano Castellano, Mérieux NutriSciences, Italy. Martin Rijkee, Handelslaboratorium Dr. A. Verwey, the Netherlands. Maurus Biedermann, Kantonales Labor Zürich, Switzerland.
This work was financed by the European Commission within the standardization mandate M/523.
ITERG, innovant par nature : Expertise, Recherche, Prestations, Production