Journal of the Brazilian Chemical Society (Jan 2006)

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

  • Marques Marlice A. S.,
  • Pereira Henrique M. G.,
  • Aquino Neto Francisco R. de

Journal volume & issue
Vol. 17, no. 2
pp. 382 – 392

Abstract

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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.

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