[Component analysis of a new anabolic androgenic steroid and its monitoring research in human urine].

A new oral drug containing an unknown anabolic androgenic steroid (AAS) was studied. The principal constituent of the unknown anabolic hormone was studied by infrared spectrum (IR), nuclear magnetic resonance spectroscopy (1H NMR), ultraviolet spectroscopy (UV), and mass spectroscopy (MS). It was inferred to be methyl-1-testosterone (M1T, 17beta-hydroxy-17alpha-methyl-5alpha-androst-1-en-3-one) which was just added to the prohibited list in 2006. In addition, a monitoring, screening and confirmation of methyl-1-testosterone was established. The detection limit (S/N = 3) was 2 ng/mL, and the limit of quantification (S/N = 10) was 10 ng/mL. The relative standard deviation was 9.8% (n = 7) for the determination of pretreated urine sample with internal standard. This method was successfully applied in the identification of M1T positive urine. The excretion curve of M1T in human urine is described. It is a significant work for the discovery, determination and monitoring of the new AAS.

[Screening, quantification and confirmation of beta-blockers in urine using gas chromatography-mass spectrometry].

A method was developed to perform the screening, quantification and confirmation of the five beta-blockers, propranolol, carteolol, bisoprolol, esmolol, and sotalol, in human urine using gas chromatography-mass spectrometry (GC-MS). In sample preparation, conjugated and unconjugated beta-blockers in urine were extracted separately, and the extracts were combined. The extracts were derivatized with N-methyl-N-trimethylsilyl-trifluoroacetamide (MSTFA) and N-methyl-bis(trifluoroacetamide) (MBTFA). The optimal conditions of GC-MS were established, and the progresses of screening by selected ion monitoring (SIM) mode and confirmation by full scan (SCAN) mode were completed. At last, the quantification curves of the five beta-blockers in spiked urine were established by SIM mode. The limits of detection were 0.2 -1.0 ng/mL. Overall recoveries were 70.5% - 103.4%, and the relative standard deviations were lower than 15%. In addition, the method was successfully applied to the analysis of the positive urine of propranolol, and the urinary excretion curve was also established accordingly. It is significant to prohibit the abuse of beta-blockers in doping control.