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The direct detection of sulfate conjugates of anabolic androgenic steroids (AAS) can be a powerful tool in doping control analysis. By skipping the solvolysis step analysis time can be reduced, and due to long term sulfate metabolites the detection time can be significantly extended as demonstrated for some AAS. This study presents the successful identification of sulfate metabolites of the doping agents oxandrolone and danazol in excretion urines by high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). The sulfate conjugate of 17β-hydroxymethyl-17α-methyl-18-nor-2-oxa-5α-androsta-13-en-3-one could be identified as a new metabolite of oxandrolone. Sulfate conjugates of the danazol metabolites ethisterone and 2α-hydroxymethylethisterone were identified in an excretion urine for the first time. In addition, these sulfate conjugates were synthesized successfully. For a confirmation analysis, the number of analytes can be increased by additional sulfate conjugates of danazol metabolites (2-hydroxymethyl-1,2-dehydroethisterone and 6β-hydroxy-2-hydroxymethylethisterone), which were also identified for the first time. The presented validation data underline the suitability of the identified sulfate conjugates for doping analysis with regard to the criteria given by the technical documents of the World Anti-Doping Agency (WADA)., (Copyright © 2016 Elsevier B.V. All rights reserved.)

A fast liquid chromatographic/mass spectrometric (LC/MS/MS) screening method for the detection, in urine, of synthetic glucocorticoids, stimulants (formoterol, modafinil and mesocarb), anti-oestrogens (finasteride, exemestane, anastrozole, letrozole and formestane) and synthetic anabolic steroids (stanozolol, gestrinone and tetrahydrogestrinone) is described. All these drugs (and/or their urinary metabolites) can be simultaneously extracted by a single liquid/liquid extraction step, at alkaline pH, after enzymatic hydrolysis with beta-glucuronidase, and assayed in 7 min by LC/MS/MS using electrospray ionization in positive ion mode and multiple reaction monitoring as the acquisition mode. All compounds show good reproducibility of both the retention times (CV% <2%) and the relative abundances (CV% <10%). The limits of detection for the anti-oestrogens, glucocorticoids and steroids are in the range of 1-30 ng/mL, and for the stimulants are in the range of 100-200 ng/mL, thus satisfying the minimum required performance limits of the World Anti-Doping Agency., (Copyright 2006 John Wiley & Sons, Ltd.)