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Sensitive and robust method for anabolic agents in human urine by gas chromatography–triple quadrupole mass spectrometry

Delgadillo, Miguel A., Garrostas, Lorena, Pozo, Óscar J., Ventura, Rosa, Velasco, Benjamín, Segura, Jordi, Marcos, Josep
Journal of chromatography 2012 v.897 pp. 85-89
chromatography, games, humans, mass spectrometry, metabolites, methyltestosterone, qualitative analysis, urine, Mexico
A rapid, sensitive and robust gas chromatography–triple quadrupole mass spectrometry method was developed for the determination of seven anabolic agents in human urine. The selection of analytes includes the main metabolites of all anabolics with higher sensitivity requirements. After optimizing the fragmentation conditions for each compound, a validation procedure for qualitative analysis was performed. The selectivity of the method showed that no interfering peaks were observed at the retention time of the compound. Adequate intermediate precision, below 14%, was observed for all of the compounds at the lower concentration tested. The concentrations assayed were in accordance with the performance limits required by the World Anti-Doping Agency (WADA). Unlike a previously published GC/QqQ method, detection of 17α-methyl-5β-androstane-3α,17β-diol (the main metabolites of methyltestosterone) at 2ng/mL was accomplished under routine conditions. The qualitative method was applied to the analysis of 1367 samples in the span of 2 weeks, as part of the doping control of the XVI Pan American Games which took place in Mexico (14th–30th October, 2011). The high sensitivity was maintained during the analysis of all analytical batches, proving for the first time the excellent ruggedness of GC/QqQ methods.