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

Journal of the Brazilian Chemical Society

Marques, Marlice A. S.¹  Aquino Neto, Francisco R. de¹  Universidade Federal do Rio de Janeiro, Rio de Janeiro, Brazil¹  Pereira, Henrique M. G.¹ 

关键词: steroids;    anabolic;    doping control;    gas chromatography;    mass spectrometry;   

DOI  :  10.1590/S0103-50532006000200024

学科分类：化学（综合）

来源: SciELO

【 摘 要 】

A procedure is described for the simultaneous determination of androgenic substances including steroids and b2-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 °C into the capillary column, initially maintained at 140 °C then programmed to 180 °C at 40 °C 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.

【 授权许可】

Unknown