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
发布时间:2018-01-08 06:05
本文关键词: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 出处:《中国运动医学杂志》2016年05期 论文类型:期刊论文
更多相关文章: 液相色谱-动态串联质谱 直接进样 刺激剂 利尿剂 兴奋剂管制
【摘要】: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。
[Abstract]:Objective: to establish and verify the simultaneous determination of 120 stimulators in human urine by liquid chromatography-dynamic tandem mass spectrometry. Methods: urine samples were precipitated with the same volume of 5% lead acetate solution and the supernatant was detected by dynamic multi-reaction monitoring mode. The detection sensitivity of traditional MRM and dynamic MRM was compared. Results: the detection limit of prohibited substances for screening was between 0.05 ng/ml and 20 ng/ml. Meet the requirements of the World Anti-Doping Agency for the ability to detect banned substances. The intra-day and inter-day precision at low, medium and high levels of concentration is less than 20%. The accuracy and matrix effect were between 80% and 120%. Conclusion: this method has high sensitivity. Dynamic MRM only scans the area near the retention time of a banned substance, and the residence time increases greatly. The detection sensitivity of dynamic MRM mode is much higher than that of traditional MRM mode. It is more suitable for simultaneous detection of many banned substances.
【作者单位】: 国家体育总局反兴奋剂中心;
【基金】:国家体育总局反兴奋剂中心科研项目(2013ZR002)
【分类号】:R872;R446.12
【正文快照】: 刺激剂和利尿剂类药物是竞技体育中经常被滥用的兴奋剂。刺激剂通过对中枢神经系统的选择性作用,能增强机体活力和敏捷性,还可使运动员疲劳感减轻,自信心增强,注意力集中。利尿剂可促进肾脏排尿功能,具有快速减轻体重的作用,主要用于需要控制体重的运动项目如拳击、摔跤、举重,
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