HPLC-MS/MS联用技术定量测定人血浆中恩替卡韦

Quantitative Determination of Entecavir in Human Plasma by HPLC-MS/MS

建立HPLC—MS／MS联用方法定量测定人血浆中恩替卡韦浓度。以地西泮为内标，甲醇为有机相，甲醇一水为（5mmol·L^-1碳酸氢铵）梯度洗脱流动相，Waters—Eterra MS-C18（2．1×50mm×5pm）色谱柱为分析柱，通过电喷雾离子源（ESI），以正离子多反应监测（MRM）方式检测。用于定量分析的离子对分别为,n／z278．2—152．1（恩替卡韦）和m／z285．0→193．0（地西泮，内标）。恩替卡韦的线性范围为0．05～20μg·L^-1，定量下限为0．05μg·L^-1（n=6）。日内、日问精密度的RSD〈15％，平均回收率〉75％。

Entecavir in human plasma was determined by high performance liquid coupled with-tandem mass spectrometry （HPLC-MS/MS）. Diazepam was used as internal standard. Entecavir was separated on a Waters-Eterra MS-C18 column（2.1 ×50 mm× 5 μm）. Electro- spray ionization（ESI） source was applied, and multiple reaction monitoring（MRM） mode was operated in the positive mode with the monitor ions at m/z 278.2→152.1 for entecavir and m/z 285.0→193.0 for the internal standard, respectively. The linear calibration curve is obtained over the concentration range of 0.05-20 μg · L^- 1. The limit of quantitation is 0.05 μg · L^-1 （n=6）. The inter and intra-day precision（RSD） is less than 15%. The average recoveries are above 75%.