Simultaneous determination of the lenalidomide,vorinostat and dexamethasone in rat plasma by LC⁃MS/MS
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摘要:
目的：建立了同时测定大鼠血浆中来那度胺、伏立诺他和地塞米松的液相色谱-质谱联用(liquid chromatography mass spectrometry，LC-MS)方法，并应用于大鼠药代动力学研究。方法：色谱柱为 Agilent Zorbax Eclipse Plus C18柱(100 mm× 2.1 mm，1.8 μm)；流动相为5 mmol/L乙酸铵+0.1%甲酸水溶液-乙腈；采用梯度洗脱；体积流量0.6 mL/min；柱温35 ℃；进样量为 5 μL；采用电喷雾离子源正离子模式(ESIp>+p> )，多反应监测进行测定。结果：来那度胺、伏立诺他和地塞米松在各自的浓度范围内检测值与浓度均具有良好的线性关系(Rp>2p> ≥0.995)，三成分的日内和日间精密度的相对标准偏差(relative standard deviation， RSD)值均小于 7.4%，准确度为 94.7%~106.7%，基质效应均在 92.3%~109.7%可接受范围内，平均提取回收率为 87.4%~ 103.6%，满足测定的要求。结论：经方法学验证，该方法可同时测定来那度胺、伏立诺他和地塞米松的血药浓度，快速、经济， 为药物研究提供了重要的分析手段。
Abstract:
Objective：A high performance liquid chromatography mass spectrometry (LC-MS) method was established to simultaneously quantify the lenalidomide，vorinostat and dexamethasone in rat plasma. The method was successfully applied to the plasma pharmacokinetics of lenalidomide，vorinostat and dexamethasone after oral administration to rats. Methods：The LC column was Agilent Zorbax Eclipse Plus C18(100 mm ×2.1 mm，1.8 μm). The mobile phase was comprised of acetonitrile and water containing 0.1% formic acid+5 mmol/L ammonium acetate. The gradient profile was used. Flow rate was 0.6 mL/min. Column temperature was 35 ℃. Sample injection volume was 5 μL. The quantification was obtained by scanning with multiple reaction monitoring(MRM)via the positive electrospray ionization(ESI + ) source. Results：The correlation coefficients of the lenalidomide，vorinostat and dexamethasone，respectively were over 0.995. The relative standard deviation(RSD)values of the inter- and intra- precisions were less than 7.4%. The accuracy ranged from 94.7% to 106.7%. The matrix effect values were sufficiently minimized to 92.3%~109.7%. The average recoveries from rat plasma were 87.4% to 103.6%. Conclusion：The validated method is further applied to the determination of lenalidomide，vorinostat and dexamethasone in plasma. The method is rapid and economical，and can provide helpful information for pharmaceutical analysis.
