液相色谱-动态串联质谱技术同时检测人尿中120种刺激剂和利尿剂等禁用物质

Mass Screening of 120 Stimulants,Diuretics and Other Prohibited Substances in Human Urine by LC-MS/MS with Dynamic MRM

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 develop a new,reliable and sensitive method for mass screening of 120 stimulants,diuretics and other prohibited substances in human urine. Method After precipitation of protein in urine with 5% Pb Ac2 aqueous solution,the supernatant was injected into LC–MS/MS system directly without sample pre-concentration. For comparison,conventional MRM（c MRM）and dynamic MRM（d MRM）acquisitions were performed under the same chromatographic conditions. Results The LC-d MRM method is fully validated and results in satisfactory limits of detection（0.05 ~20 ng/m L）. The intra- and inter-day precisions（% CV）in low,moderate and high concentration levels are all less than 20%. The method also affords satisfactory results in terms of accuracy（80% ~120%）,matrix effect（80% ~120%）and specificity.Conclusions The LC-d MRM method reveals high sensitivity,accuracy,and reproducibility.