Improvements in steroid screening in doping control with special emphasis to GC-MS analytical conditions and method validation

Abstract

A procedure is described for the simultaneous determination of androgenic substances including steroids and beta2-agonists. The method involves analysis of hydrolized urinary anabolic compounds using liquid-liquid extraction, with subsequent conversion to trimethylsilylether derivatives for the analysis by GC-MS. Pulse split injection 1/10 of the TMS derivatives at 280 degreesC into the capillary column, initially maintained at 140 degreesC then programmed to 180 degreesC at 40 degreesC min-1, followed by 3 ºC min-1 to 230 ºC and then 40 ºC min-1 to 300 ºC, resulted in good resolution and peak shape for all compounds. The detection limits of most of the steroids were 1 ng mL-1 except for formebolone and trenbolone (25 ng mL-1). When applied to selected urine samples with evidence of bacterial degradation and metabolites from usual medications/vitamins, the method allowed rapid screening for androgens and other substances monitored in routine. The resolution was adequate to evaluate the endogenous steroid profile relevant to doping control and medical applications.

Keywords

• steroids
• anabolic
• doping control
• gas chromatography
• mass spectrometry