Liu Mingyuan, Zhang Dan, Sun Yantong, Wang Yingwu, Liu Zeyuan, Gu Jingkai
Research Center for Drug Metabolism, College of Life Science, Jilin University, Changchun 130023, People's Republic of China.
Biomed Chromatogr. 2007 May;21(5):508-13. doi: 10.1002/bmc.785.
An analytical method for the determination of bisoprolol in human plasma has been developed based on liquid chromatography-tandem mass spectrometry (LC-MS/MS). The analyte and internal standard (IS) diphenhydramine were cleaned up by protein precipitation with acetonitrile, reconstituted in mobile phase and separated by reversed-phase high-performance liquid chromatography (HPLC) using methanol:10 mm ammonium acetate:formic acid (70:30:0.1 v/v/v) as mobile phase. Detection was carried out by multiple reaction monitoring (MRM) on an LC-MS/MS system and was completed within 2.5 min. The assay was linear over the range 0.5-100 ng/mL with a limit of quantitation (LOQ) of 0.5 ng/mL. The intra- and inter-day precision levels were within 5.54 and 9.95%, respectively, while the accuracy was in the range 89.4-113%. This method has been utilized in a pharmacokinetic study, where healthy volunteers were treated with an oral dose of 5 mg bisoprolol.
已开发出一种基于液相色谱 - 串联质谱法(LC-MS/MS)测定人血浆中比索洛尔的分析方法。分析物和内标(IS)苯海拉明通过用乙腈进行蛋白沉淀来净化,在流动相中复溶,并使用甲醇:10 mM乙酸铵:甲酸(70:30:0.1 v/v/v)作为流动相通过反相高效液相色谱(HPLC)进行分离。在LC-MS/MS系统上通过多反应监测(MRM)进行检测,并在2.5分钟内完成。该测定法在0.5 - 100 ng/mL范围内呈线性,定量限(LOQ)为0.5 ng/mL。日内和日间精密度水平分别在5.54%和9.95%以内,而准确度在89.4 - 113%范围内。该方法已用于一项药代动力学研究,其中健康志愿者口服5 mg比索洛尔进行治疗。