Laboratorio Antidoping, Federazione Medico Sportiva Italiana, Largo G. Onesti 1, 00197 Rome RM, Italy.
Rapid Commun Mass Spectrom. 2010 May 30;24(10):1475-80. doi: 10.1002/rcm.4542.
A fast method has been developed for the simultaneous determination of 52 stimulants and narcotics excreted unconjugated in urine by gas chromatography/mass spectrometry (GC/MS). The procedure involves the liquid/liquid extraction of the analytes from urine at strong alkaline pH and the injection of the extract into a GC/MS instrument with a fast GC column (10 m x 0.18 mm i.d.); the short column allows the complete separation of the 52 analytes in a chromatographic run of 8 min. The method has been fully validated giving lower limits of detection (LLODs) satisfactory for its application to antidoping analysis as well as to forensic toxicology. The repeatability of the concentrations and the retention times are good both for intra- and for inter-day experiments (%CV of concentrations always lower than 15 and %CV of retention times lower than 0.6). In addition, the analytical bias is satisfactory (A% always >15%). The method proposed here would be particularly useful whenever there are time constraints and the analyses have to be completed in the shortest possible time.
已开发出一种快速方法,可通过气相色谱/质谱法(GC/MS)同时测定未经结合排泄在尿液中的 52 种兴奋剂和麻醉品。该方法涉及在强碱性 pH 下从尿液中用液/液萃取分析物,然后将萃取物注入具有快速 GC 柱(10 m x 0.18 mm id)的 GC/MS 仪器中;短柱允许在 8 分钟的色谱运行中完全分离 52 种分析物。该方法已得到充分验证,其检测限(LLOD)足以满足反兴奋剂分析和法医毒理学的要求。无论是在日内还是日间实验中,浓度和保留时间的重复性都很好(浓度的 CV%始终低于 15%,保留时间的 CV%低于 0.6%)。此外,分析偏差令人满意(A%始终>15%)。当时间紧迫且必须在尽可能短的时间内完成分析时,这里提出的方法特别有用。