Doping Control Center, Korea Institute of Science and Technology, Seoul, Korea.
Anal Bioanal Chem. 2011 Sep;401(4):1353-63. doi: 10.1007/s00216-011-5210-1. Epub 2011 Jul 10.
A sensitive and rapid method based on liquid chromatography-triple-quadrupole tandem mass spectrometry (LC-MS/MS) with electrospray ionization (ESI) has been developed and validated for the screening and confirmation of 44 exogenous anabolic steroids (29 parent steroids and 15 metabolites) in human urine. The method involves an enzymatic hydrolysis, liquid-liquid extraction, and detection by LC-MS/MS. A triple-quadrupole mass spectrometer was operated in positive ESI mode with selected reaction monitoring (SRM) mode for the screening and product ion scan mode for the confirmation. The protonated molecular ions were used as precursor ions for the SRM analysis and product ion scan. The intraday and interday precisions of the target analytes at concentrations of the minimum required performance levels for the screening were 2-14% and 2-15%, respectively. The limits of detection for the screening and confirmation method were 0.1-10 ng/mL and 0.2-10 ng/mL, respectively, for 44 steroids. This method was successfully applied to analysis of urine samples from suspected anabolic steroid abusers.
一种基于液相色谱-串联三重四极杆质谱（LC-MS/MS）联用电喷雾电离（ESI）的灵敏、快速方法已经建立并验证，用于筛选和确证人尿液中的 44 种外源性合成代谢类固醇（29 种母体类固醇和 15 种代谢物）。该方法包括酶解、液液萃取和 LC-MS/MS 检测。三重四极杆质谱仪以正电喷雾模式（ESI）操作，采用选择反应监测（SRM）模式进行筛选，采用产物离子扫描模式进行确证。质子化分子离子被用作 SRM 分析和产物离子扫描的前体离子。在最低性能水平浓度下，目标分析物的日内和日间精密度分别为 2-14%和 2-15%。筛选和确证方法的检测限分别为 0.1-10 ng/mL 和 0.2-10 ng/mL，适用于 44 种类固醇。该方法已成功应用于疑似合成代谢类固醇滥用者尿液样本的分析。
