Urinary signature of anabolic steroids and glucocorticoids in humans by LC-MS

A metabonomic strategy based on LC-MS was employed to investigate the metabolic profile of urine samples from 20 athletes who had been tested positive for corticoids and anabolic steroids and 29 controls. In this aim, different sample preparations and chromatographic conditions were compared. The acquired LC-MS data of doped athletes and controls were subjected to analysis of variance (ANOVA) and principal component analysis (PCA). Using this approach, molecular signature of human urine was obtained showing that metabonomics could be a complementary tool to discriminate different urinary profiles and to track down metabolic changes in humans.     

Multiresidue analysis of anabolic compounds in bovine hair by gas chromatography-tandem mass spectrometry

A rapid and specific multiresidue method was developed to perform screening and confirmation of 15 anabolics steroids in bovine hair, namely: dienestrol, DES, hexestrol, 17α- and 17β-estradiol, 17α- and 17β-19-nortestosterone, 17α- and 17β-boldenone, testosterone (β) and epitestosterone (α), ethynylestradiol, α-methyltestosterone, and α- and β-Zearalanol.After methanolic and solid-phase extraction, trimethylsilyl derivatization (TMS) was performed and the derivatized extracts submitted to GC-MS-MS analysis. TMS derivatives of the studied hormones yielded specific MS-MS fragmentation with a high abundance for ions selected in the screening procedure.Validation was performed regarding qualitative parameters: decision limit (CCα), detection capability (CCβ) and specificity. For confirmation, European union criteria 2002/657/EC were considered. Detection capability ranged between 1.0 and 10.0 ng g⁻¹ depending on the compound.