Fast screening of anabolic steroids and other banned doping substances in human urine by gas chromatography/tandem mass spectrometry.
A fast and sensitive method for the comprehensive screening of anabolic agents and other banned doping substances using gas chromatography/tandem mass spectrometry (GC/MS/MS) with an external ionization ion trap mass spectrometer is presented. The method takes advantage of the resolving power of MS/MS to eliminate background interferences, thus speeding up the chromatographic analysis. For each compound, different fragmentation reactions were studied and their collision energies optimized to obtain the best sensitivity in terms of their signal-to-noise ratio (S/N). A dramatic reduction in overall analysis time was achieved compared with other common approaches. More than 50 substances could finally be monitored in less than 7.4 min with detection limits (S/N >3) lower than 0.5 ng ml(-1) for most of the compounds with special sensitivity requirements according to the International Olympic Committee (IOC). 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 analytes. Good intermediate precision, below 25% for most of the compounds, and robustness were observed. The optimized method was successfully applied to analyse more than 100 real human urine samples with optimum sensitivity and specificity rates.
Marcos
J
J
Pharmacology Research Unit, Institut Municipal d'Investigació Mèdica, IMIM, Department of Experimental and Health Sciences, Universitat Pompeu Fabra, Dr. Aiguader 80, 08003 Barcelona, Spain.
Pascual
J A
JA
de la Torre
X
X
Segura
J
J
D045930:Anabolic Agents / Q000652:urine*; D001711:Biotransformation; D004300:Doping in Sports; D004845:Epitestosterone / Q000652:urine; D008401:Gas Chromatography-Mass Spectrometry; D005966:Glucuronidase / Q000737:chemistry; D006801:Humans; D007202:Indicators and Reagents; D011786:Quality Control; D012015:Reference Standards; D015203:Reproducibility of Results; D015813:Substance Abuse Detection / Q000379:methods*; D013739:Testosterone / Q000652:urine
D045930:Anabolic Agents; D007202:Indicators and Reagents; D013739:Testosterone; D004845:Epitestosterone; D005966:Glucuronidase