HPLC-MS法测定人血浆中异丁司特浓度

Determination of ibudilast in human plasma by HPLC-MS

目的:建立HPLC-MS法测定人血浆中异丁司特的浓度。方法:以非那西丁为内标,色谱条件:Lichro-spher C18色谱柱(250mm×4.6mm,5μm),以0.5%乙酸水-甲醇(20:80)为流动相,流速为1.0mL·min-1,质谱检测。结果:异丁司特在2-200ng·mL-1范围内线性关系良好(r=0.999 7),最低定量浓度为1.0ng·mL-1。方法平均回收率为99.37%,提取回收率均大干95%,日内与日间RSD均小于5%。结论:本法快速简便、灵敏准确,适宜人血浆中异丁司特的浓度测定。

Objective:To develop a HPLC-MS method for determination of ibudilast in human plasma. Methods: Phenacetin was used as an internal standard and the chromatographic conditions adopted were:Lichrospher C18 column(250mm×4.6mm,5μm) ,a mobile phase of 0.5% acetic acid-methanol(20:80) with a flow rate of 1.0mL·min-1, using a single quadrapole MS as detector, Re-sults: Ibudilast had a good linear range of 2-200ng·mL-1 ( r = 0.999 7) with a detection limit of 1.0 ng·mL-1. The average recovery was 99.37 % with an extraction recovery of more than 95 % . RSD was less than 5% for intra-day and inter-day assay. Conclusion: The method established is simple, rapid, sensitive,accurate and suitable for determination of ibudilast in human plasma.