Liu Gang-Yi, Wang Wei, Jia Jing-Ying, Lu Chuan, Liu Yan-Mei, Zhang Meng-Qi, Liu Yun, Li Shui-Jun, Yu Chen
Central Laboratory, Shanghai Xuhui Central Hospital,966 Huaihai Middle Road, Shanghai 200031, China.
Biomed Chromatogr. 2010 Jun;24(6):574-80. doi: 10.1002/bmc.1329.
A simple, reliable and sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) protocol was developed and validated for quantification of bisoprolol in human plasma. The sample was pretreated with a simple procedure of protein precipitation and an isotope-labeled d5-bisoprolol was used as internal standard. The chromatographic separation was performed on a Capcell Pak C(18) MG III column (100 mm x 2.0 mm, 5 microm). The protonated ion of the analyte was detected in positive ionization by multiple reaction monitoring mode. The mass transition pairs of m/z 326.3 --> 116.3 and m/z 331.3 --> 121.3 were used to detect bisoprolol and the internal standard, respectively. Linearity, accuracy, precision, recovery, matrix effect, dilution test and stability were evaluated during method validation over the range of 0.5-100 ng/mL. The validated method was successfully applied to analyze human plasma samples in a bisoprolol bioavailability study.
开发并验证了一种简单、可靠且灵敏的液相色谱串联质谱（LC-MS/MS）方法，用于定量测定人血浆中的比索洛尔。样品采用简单的蛋白质沉淀程序进行预处理，并使用同位素标记的d5-比索洛尔作为内标。色谱分离在Capcell Pak C(18) MG III柱（100 mm×2.0 mm，5微米）上进行。在正离子模式下通过多反应监测模式检测分析物的质子化离子。分别使用m/z 326.3 --> 116.3和m/z 331.3 --> 121.3的质量转移对来检测比索洛尔和内标。在方法验证过程中，在0.5-100 ng/mL范围内评估了线性、准确度、精密度、回收率、基质效应、稀释试验和稳定性。该验证方法成功应用于比索洛尔生物利用度研究中的人血浆样品分析。
