论文部分内容阅读
目的建立测定人血浆中乌苯美司的液相色谱-串联质谱(LC-MS/MS)方法。方法采用Inertsil ODS-3(50mm×2.1mm,5μm)色谱柱,流动相为甲醇-20mmol·L-1甲酸铵(含0.05%甲酸)(50∶50,V/V),流速:0.3mL·min-1;质谱仪离子源为电喷雾离子源(ESI),正离子模式检测,监测离子为309.55→119.88(乌苯美司)和339.25→280.8(溴莫普林,内标)。结果乌苯美司在2～3000μg·L-1线性关系良好(r=0.9982),定量限为2μg·L-1。主要药动学参数分别为:ρmax(2702±s431)μg·L-1,tmax(0.58±0.26)h,t虔蚝α(0.53±0.17)h,t虔蚝β(1.9±0.5)h,AUC0～t(3744±574)μg·h·L-1,Vc/F(0.0080±0.0020)L,CL(0.0082±0.0012)L·h-1。结论本方法操作简便、准确、灵敏,适用于乌苯美司的人体药动学研究。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of ubenimex in human plasma. Methods Inertsil ODS-3 (50mm × 2.1mm, 5μm) column was used. The mobile phase was methanol-20mmol·L-1 ammonium formate with 0.05% formic acid (50:50, V / V) min-1. The mass spectrometer ion source was electrospray ionization source (ESI) with positive ion mode detection. The monitored ions were 309.55 → 119.88 (ubenimex) and 339.25 → 280.8 (bromopram, internal standard). Results Ubenimex had good linearity (r = 0.9982) at 2 ~ 3000μg · L-1, and the limit of quantification was 2μg · L-1. The main pharmacokinetic parameters were ρmax (2702 ± s431) μg · L-1, tmax (0.58 ± 0.26) h, t ± 0.23 ± 0.17 h and t ± 1.9 ± 0.5 h, AUC0 ~ t (3744 ± 574) μg · h · L-1, Vc / F (0.0080 ± 0.0020) L, CL (0.0082 ± 0.0012) L · h-1. Conclusion The method is simple, accurate and sensitive and is suitable for the study of human pharmacokinetics of ubenimex.