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目的:建立测定人血浆中氨溴索浓度的高效液相色谱串联质谱法,以用于氨溴索人体药动学研究。方法:以西替利嗪为内标,血浆样品经乙腈沉淀后,经HPLC-MS/MS分离-分析。采用Waters ODS C_(18)柱(50 mm×2.1 mm,3.5μm),以甲醇:5mmol·L~(-1)乙酸铵(72.5:27.5)为流动相,流速:0.20 ml·min~(-1),采用电喷雾离子源(ESI),以多离子反应监测方式(MRM)进行正离子监测,氨溴索和内标西替利嗪的定量分析离子对分别为m/z 379.0→263.9和m/z 389.1→201.3。结果:氨溴索血浆浓度测定方法线性范围为1.99～398 ng·ml~(-1),r=0.999 0。定量下限为1.99 ng·ml~(-1),方法回收率在85%～115%之间。日内和日间RSD<15%。结论:本法灵敏、准确、可靠,适用于盐酸氨溴索人体药动学研究。
OBJECTIVE: To establish a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for the determination of ambroxol in human plasma for human ambroxol pharmacokinetic study. Methods: Cetirizine was used as an internal standard. The plasma samples were separated by acetonitrile-acetonitrile and analyzed by HPLC-MS / MS. The mobile phase consisted of Waters ODS C 18 column (50 mm × 2.1 mm, 3.5 μm) and methanol (5 mmol·L -1) ammonium acetate (72.5: 27.5) at a flow rate of 0.20 ml · min -1 1). The electrospray ionization source (ESI) was used for positive ion monitoring in the multi-ion reaction monitoring mode (MRM). The ion pairs of ambroxol and internal standard cetirizine were m / z 379.0 → 263.9 and m / z 389.1 → 201.3. Results: The linear range of ambroxol plasma concentration was 1.99 ~ 398 ng · ml ~ (-1), r = 0.999 0. The lower limit of quantification was 1.99 ng · ml -1, and the recovery rate was between 85% and 115%. Day and day RSD <15%. Conclusion: This method is sensitive, accurate and reliable and is suitable for the study of human ambroxol hydrochloride pharmacokinetics.