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高效液相色谱/轨道阱质谱法作为兴奋剂检测筛选方法的介绍。

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

作者信息

Virus E D, Sobolevsky T G, Rodchenkov G M

机构信息

Moscow Antidoping Center, Elizavetynsky10, 105005, Moscow, Russia.

出版信息

J Mass Spectrom. 2008 Jul;43(7):949-57. doi: 10.1002/jms.1447.

Abstract

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 1 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.

摘要

已开发出一种新的兴奋剂控制筛查方法,用于分析人尿中的兴奋剂,该方法采用具有源内碰撞诱导解离和大气压化学电离的高效液相色谱/轨道阱质谱联用技术。所开发的方法能够检测29种化合物,包括具有抗雌激素活性的药物、β₂激动剂、外源性合成代谢类固醇以及其他合成代谢药物。使用外部参比时,该方法的质量准确度在2 ppm时更佳。所有测试化合物的检测限均优于100 pg/ml。大多数分析物的回收率高于70%。该方法中所包含的兴奋剂在浓度为1和10 ng/ml时的测量中位重复性值分别为21%和17%。日内精密度(n = 6)的相对标准偏差(RSD)范围为RSD = 16 - 22%,而日间精密度(n = 18)的相对标准偏差范围为RSD = (17 - 26%),具体取决于所研究的溶质浓度。

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