HPLC-MS/MS联用技术定量测定人血浆中恩替卡韦

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-水为(5 mmol.L-1碳酸氢铵)梯度洗脱流动相,Waters-Eterra MS-C18(2.1×50 mm×5μm)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m/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、日间精密度的RSD15%,平均回收率75%。

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

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). Electrospray 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%.