液相色谱-串联质谱法测定人血浆中拉米夫定浓度

 目的 试图建立测定人血浆中拉米夫定浓度的液相色谱-串联质谱法.方法 以吉西他滨为内标,内标法定量.流动相:甲醇-10 mmol/L乙酸铵(12: 88,v/v);质谱采用离子喷雾离子源,扫描方式为多反应监测(MRM),用于定量分析的离子反应分别为m/z 230m/z 111.9(拉米夫定)和m/z 263.8m/z 111.9(吉西他滨);药动学参数采用DAS2.0软件处理获得.结果 拉米夫定和内标吉西他滨的保留时间分别为2.9 min和2.4 min;拉米夫定的线性范围为0.0100~2.0000 μg/ml ,r=0.9996,回归方程:Y=0.0032X+0.0003,最低检测浓度为0.0100 μg/ml;提取回收率为95%～105%范围内;日内日间精密度RSD<6%.结论 此法适合人体血浆拉米夫定浓度的监测及生物利用度研究,结果准确、可靠.

Determination of lamivudine in healthy volunteers' plasma by LC/MS/MS

Objective To establish an LC/MS/MS method for the determination of lamivudine. Methods Gemcitabine was set as an internal standard. The mobile phase was a mixture of anmnmium -methanol （88：12）. Electronic spray ionization （ESI） and multiple/reaction monitoring （MRM） were used for the determination of lamivudine. The analysis was performed in the selected ion monitoring mode at m/z 111.9 for lamivudine and m/z 111.9 for gemcitabine. Pharmaeokinetic parameters were obtained using DAS 2.0 program. Results The retention time of lainivudine and gemcitabine was observed at 2.9 rain and 2.4 min,respectively. The linear response for lamivudine was obtained in the range of 0.01 -2.00 μg/ml with a correlation coefficient of 0. 9996. The limit of quantifi- cation was 0.01 μg/ml . Precision of either intra - day or inter - day assay was less than 6.0% and the exaction recovery was between 95% and 105%. Conclusions The assay method we used is precise and accurate enough to determine the amount of lamivudine and its bioavailability in human plasma.