Guangzhou Institute of Biomedicine and Health, Chinese Academy of Sciences, Guangzhou 510663, PR China.
J Pharm Biomed Anal. 2010 Jun 5;52(2):227-31. doi: 10.1016/j.jpba.2009.12.020. Epub 2009 Dec 28.
A chiral liquid chromatography-tandem mass spectrometry (LC-MS/MS) simultaneous stereoselective analysis of bambuterol and its active metabolite terbutaline enantiomers in Wistar rat plasma has been developed and validated. All analytes and the internal standard were extracted from rat plasma samples by liquid-liquid extraction, separated on macrocyclic glycopeptide teicoplanin column with mobile phase constituted of 20mM ammonium acetate solution-methanol (10:90, v/v) at a flow-rate of 0.4 mL/min. Detection was performed on an API 3000 tandem mass spectrometer with positive electrospray ionization in multiple reaction monitoring mode. The calibration curves in the range 1-800 ng/mL were linear and the accuracy for each analyte was within 8.0%. The intra- and inter-day precision as determined from quality control samples was less than 10.1%. The validated assay was successfully used to determine the enantiomers of bambuterol and terbutaline in rat plasma samples in the pharmacokinetic studies of rac-bambuterol.
建立并验证了一种手性液相色谱-串联质谱（LC-MS/MS）法，用于同时立体选择性分析 Wistar 大鼠血浆中的班布特罗及其活性代谢物特布他林对映体。所有分析物和内标均通过液-液萃取从大鼠血浆样品中提取，采用大环糖肽替考拉宁柱，以 20mM 乙酸铵溶液-甲醇（10:90，v/v）为流动相，流速为 0.4mL/min 进行分离。采用 API 3000 串联质谱仪，正电喷雾电离，多反应监测模式进行检测。在 1-800ng/mL 范围内，校准曲线呈线性，每种分析物的准确度均在 8.0%以内。从质控样品中确定的日内和日间精密度小于 10.1%。该验证后的分析方法成功用于 rac-班布特罗药代动力学研究中大鼠血浆样品中班布特罗和特布他林对映体的测定。
