title: Ultra-high performance liquid chromatography-tandem mass spectrometry in high-throughput confirmation and quantification of 34 anabolic steroids in bovine muscle.
abstract: An ultra-high performance liquid chromatography tandem mass spectrometry multi-residue method for the determination of 34 anabolic steroids (10 estrogens including stilbenes, 14 androgens and 10 gestagens) in meat of bovine origin is reported. The extraction and clean-up procedure involved homogenization with methanol, defatting with hexane, liquid/liquid extraction with diethylether and finally SPE clean-up with coupled Si and NH(2) cartridges. The analytes were separated on a 1.9 μm Hypersil Gold column (100×2.1 mm) and quantified on a triple quadrupole mass spectrometer (TSQ Vantage) operating simultaneously in both positive and negative atmospheric pressure chemical ionisation (APCI) modes. This analytical procedure was subsequently validated according to EU criteria (CD 2002/657/EC), resulting in decision limits and detection capabilities ranging between 0.04 and 0.88 μg kg(-1) and 0.12 and 1.9 μg kg(-1), respectively. The method obtained for all, natural and synthetic steroids, adequate precisions and intra-laboratory reproducibilities (relative standard deviation below 20%), and the linearity ranged between 0.991 and 0.999. The performance characteristics fulfill the recommended concentrations fixed by the Community Reference Laboratories. The developed analysis is sensitive, and robust and therefore useful for confirmation and quantification of anabolic steroids for research purposes and residue control programs.
authors: Ghent University, Faculty of Veterinary Medicine, Research Group Veterinary Public Health and Zoonoses, Department of Veterinary Public Health and Food Safety, Merelbeke, Belgium. Lynn.Vanhaecke@UGent.be
authors: Lynn
authors: L
authors: Vanhaecke
authors: Julie
authors: J
authors: Vanden Bussche
authors: Klaas
authors: K
authors: Wille
authors: Karen
authors: K
authors: Bekaert
authors: Hubert F
authors: HF
authors: De Brabander
mesh_terms: D045930:Anabolic Agents / Q000032:analysis* / Q000302:isolation & purification; D000818:Animals; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006586:Hexanes / Q000737:chemistry; D008460:Meat / Q000032:analysis*; D000432:Methanol / Q000737:chemistry; D052616:Solid Phase Extraction / Q000379:methods; D013256:Steroids / Q000032:analysis* / Q000302:isolation & purification; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D045930:Anabolic Agents; D006586:Hexanes; D013256:Steroids; D000432:Methanol