Determination of Hormones Residues in Milk by Gas Chromatography-Mass Spectrometry |
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Authors: | Iwona Matraszek-Zuchowska Barbara Wozniak Andrzej Posyniak |
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Affiliation: | 1.Department of Pharmacology and Toxicology,National Veterinary Research Institute,Pulawy,Poland |
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Abstract: | The article presents the use of gas chromatography-mass spectrometry (GC-MS) technique in a method for the determination of 18 anabolic hormones from synthetic stilbenes, steroids and resorcylic acid lactones (RALs) groups in raw milk and milk powder. Sample preparation consisted of liquid-liquid extraction with diethyl ether and purification by solid phase extraction (SPE). Prior to instrumental analysis, the reaction of derivatisation with the heptafluorobutyric anhydride or N-methyl-N-trimethylsilyltrifluoroacetamide was performed. Method validation was carried out according to the required performance criteria of the Commission Decision 2002/657/EC. The apparent recovery of all analytes at 1 μg L?1 (kg?1) level was ranged between 70.4 and 119.4 % with the coefficients of variation values less than 30 %. The decision limits (CCα) and the detection capabilities (CCβ) were in the range of from 0.11 to 0.44 μg L?1 (kg?1) and from 0.19 to 0.75 μg L?1 (kg?1), respectively. The procedure has been accredited and successfully applied as a screening method for the presence of hormone residues in the study of commercial samples of milk. |
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