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Introduction of HPLC/orbitrap mass spectrometry as screening method for doping control

机译:引入HPLC / orbitrap质谱法作为掺杂控制的筛选方法

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摘要

A new doping control screening method has been developed, for the analysis of doping agents in human urine, using HPLC/orbitrap with in-source collision-induced dissociation and atmospheric pressure chemical ionization. The developed method allows the detection of 29 compounds, including agents with antiestrogenic activity, beta(2) agonists,exogenous anabolic steroids, and other anabolic agents. The mass accuracy of this method is better at 2 ppm using an external reference. The detection limit for all compounds tested was better than 100 pg/ml. The recoveries of most analytes were above 70%. The measured median repeatability values for doping agents included in the method at concentrations of I and 10 ng/ml were 21 and 17%, respectively. The relative standard deviation (RSD) of the intraday precision (n = 6) ranged from RSD = 16-22%, whereas the interday precision (n = 18), ranged from RSD = 17-26%, depending on the solute concentration investigated.
机译:已经开发了一种新的掺杂控制筛选方法,该方法使用HPLC / orbitrap以及源内碰撞诱导的离解和大气压化学电离来分析人尿中的掺杂剂。开发的方法允许检测29种化合物,包括具有抗雌激素活性的药物,β(2)激动剂,外源性合成代谢类固醇和其他合成代谢剂。使用外部参考,此方法的质量精度在2 ppm时更好。所有测试化合物的检出限均优于100 pg / ml。大多数分析物的回收率均在70%以上。在I和10 ng / ml的浓度下,该方法中所含掺杂剂的测量中值重复性值分别为21%和17%。盘中精度(n = 6)的相对标准偏差(RSD)为RSD = 16-22%,而盘中精度(n = 18)的相对标准偏差(RSD)为17-26%,具体取决于所研究的溶质浓度。

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