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目的:采用液相色谱-动态串联质谱技术,建立和验证同时检测人尿样中120种刺激剂、利尿剂和其它禁用物质的方法。方法:尿样经同等体积的5%醋酸铅水溶液沉淀蛋白质后,上清液用动态多反应监测模式(d MRM)进行检测,并比较了传统MRM与动态MRM在检测灵敏度上的差异。结果:所筛查禁用物质的检测限均介于0.05~20 ng/ml之间,达到世界反兴奋剂机构对禁用物质检测能力的要求。在低、中和高三个浓度级别的日内和日间精密度均小于20%,准确度和基质效应在80%~120%之间。结论:该方法具有灵敏度高、准确可靠和重现性好等特点。动态MRM模式只扫描某个禁用物质保留时间附近区域,驻留时间大大增加,其检测灵敏度远高于传统MRM模式,更适合于多种禁用物质的同时检测。
OBJECTIVE: To establish and validate simultaneous detection of 120 stimulants, diuretics and other banned substances in human urine samples by liquid chromatography-tandem mass spectrometry. Methods: After the urine samples were precipitated with the same volume of 5% aqueous lead acetate solution, the supernatants were detected by d MRM. The differences of detection sensitivity between traditional MRM and dynamic MRM were also compared. Results: The detection limits of the banned substances tested ranged from 0.05 to 20 ng / ml, meeting the requirements of the World Anti-Doping Agency for banned substances detection. The intra- and inter-day precision was less than 20% in the three levels of low, middle and high concentration, and the accuracy and matrix effects were between 80% and 120%. Conclusion: This method has the characteristics of high sensitivity, accuracy and reliability and reproducibility. The dynamic MRM mode only scans the area near the retention time of a prohibited substance and greatly increases the residence time. The detection sensitivity is much higher than the traditional MRM mode, which is more suitable for the simultaneous detection of many prohibited substances.