Georgakopoulos Costas G, Vonaparti Ariadni, Stamou Marianna, Kiousi Polyxeni, Lyris Emmanouil, Angelis Yiannis S, Tsoupras George, Wuest Bernhard, Nielen Michel W F, Panderi Irene, Koupparis Michalis
Doping Control Laboratory of Athens, Olympic Athletic Center of Athens Spiros Louis, 37 Kifissias Ave., 151 23 Maroussi, Greece.
Rapid Commun Mass Spectrom. 2007;21(15):2439-46. doi: 10.1002/rcm.3103.
A new combined doping control screening method for the analysis of anabolic steroids in human urine using liquid chromatography/electrospray ionization orthogonal acceleration time-of-flight mass spectrometry (LCoaTOFMS) and gas chromatography/electron ionization orthogonal acceleration time-of-flight mass spectrometry (GCoaTOFMS) has been developed in order to acquire accurate full scan MS data to be used to detect designer steroids. The developed method allowed the detection of representative prohibited substances, in addition to steroids, at concentrations of 10 ng/mL for anabolic agents and metabolites, 30 ng/mL for corticosteroids, 500 ng/mL for stimulants and beta-blockers, 250 ng/mL for diuretics, and 200 ng/mL for narcotics. Sample preparation was based on liquid-liquid extraction of hydrolyzed human urine, and the final extract was analyzed as trimethylsilylated derivatives in GCoaTOFMS and underivatized in LCoaTOFMS in positive ion mode. The sensitivity, mass accuracy, advantages and limitations of the developed method are presented.
为了获取准确的全扫描质谱数据以用于检测设计类固醇，已开发出一种新的联合兴奋剂控制筛查方法，该方法使用液相色谱/电喷雾电离正交加速飞行时间质谱法（LCoaTOFMS）和气相色谱/电子电离正交加速飞行时间质谱法（GCoaTOFMS）来分析人尿中的合成代谢类固醇。除类固醇外，所开发的方法还能检测出代表性的违禁物质，其检测浓度分别为：合成代谢剂和代谢物10 ng/mL、皮质类固醇30 ng/mL、兴奋剂和β受体阻滞剂500 ng/mL、利尿剂250 ng/mL、麻醉品200 ng/mL。样品制备基于水解人尿的液-液萃取，最终提取物在GCoaTOFMS中以三甲基硅烷化衍生物形式进行分析，在LCoaTOFMS中以正离子模式进行非衍生化分析。文中介绍了所开发方法的灵敏度、质量准确性、优点和局限性。
