Huang Jinchang, Xu Yu, Gao Shu, Rui Lei, Guo Qingxiang
Department of Chemistry, University of Science and Technology of China, Hefei 230026, China.
Rapid Commun Mass Spectrom. 2005;19(16):2321-4. doi: 10.1002/rcm.2066.
A simple and sensitive liquid chromatography/tandem mass spectrometry method, employing electrospray ionization, has been developed and validated to quantify rabeprazole in human plasma using omeprazole as the internal standard. The method was validated to demonstrate the specificity, lower limit of quantification, accuracy, and precision of measurements. Selected reaction monitoring was specific for rabeprazole and omeprazole (the internal standard, IS); no endogenous materials interfered with the analysis of rabeprazole and IS from blank plasma. The assay was linear over the concentration range 0.2-200 ng/mL using a 2 microL aliquot of plasma. The correlation coefficients for the calibration curves ranged from 0.9988-0.9994. The intra- and inter-day precision, calculated from quality control samples, were less than 6.65%. A mixture of methanol and water (50:50) was used as the isocratic mobile phase, with 0.1% of formic acid in water, that did not affect the stability of rabeprazole or IS. A simple sample preparation method of protein precipitation with methanol was chosen. The method was employed in a pharmacokinetic study after oral administration of 20 mg rabeprazole to 24 healthy volunteers.
已开发并验证了一种采用电喷雾电离的简单且灵敏的液相色谱/串联质谱法，以奥美拉唑为内标定量测定人血浆中的雷贝拉唑。该方法经过验证，以证明测量的特异性、定量下限、准确性和精密度。选择反应监测对雷贝拉唑和奥美拉唑（内标，IS）具有特异性；没有内源性物质干扰空白血浆中雷贝拉唑和内标的分析。使用2微升血浆等分试样，该测定在0.2 - 200纳克/毫升的浓度范围内呈线性。校准曲线的相关系数范围为0.9988 - 0.9994。由质量控制样品计算得出的日内和日间精密度均小于6.65%。甲醇和水（50:50）的混合物用作等度流动相，水中含有0.1%的甲酸，这不会影响雷贝拉唑或内标的稳定性。选择了用甲醇进行蛋白沉淀的简单样品制备方法。该方法用于对24名健康志愿者口服20毫克雷贝拉唑后的药代动力学研究。
