LC-MS/MS内标法测定人血浆中西地那非的浓度  

Determination of sidenafil concentration in human plasma by LC-MS/MS with internal standard method

作　　者：邓晓兰[1] 谭志荣[1] 陈尧[1] 李慧[1] 王医成[1] 黄琪[2] 欧阳冬生[1] 

机构地区：[1]中南大学临床药理研究所湖南省遗传药理学重点实验室 [2]中南大学药学院

出　　处：《中国临床药理学与治疗学》2011年第11期1272-1277,共6页Chinese Journal of Clinical Pharmacology and Therapeutics

摘　　要：目的:建立LC-MS/MS法检测人血浆中西地那非的浓度。方法:以地西泮为内标,血浆样品经MTBE液液萃取后,采用Waters XTerraMS C18(150mm×2.1mm,5μm)柱分离,流动相为甲醇:10mmol/L醋酸铵=85∶15(V/V),流速为0.30mL/min。然后采用电喷雾离子源(ESI源)正离子多反应监测(MRM)扫描分析,西地那非和内标地西泮的离子选择通道分别为:m/z475.3→58.1和285.5→154.0。结果:西地那非的线性范围为1.50～765.90ng/mL,最低检测浓度为1.50ng/mL,日内和日间变异均<15%。结论:本法适用于西地那非的人体药物代谢动力学研究。AIM：To establish an LC-MS/MS method for determining the concentration of sildenafil in human plasma.METHODS： Diazepam was used as internal standard,the plasma samples extracted by MTBE were separated on a Waters XTerra MS C18 column（150 mm×2.1 mm,5 μm） with mobile phase contained methanol and 10 mmol/L Ammonium acetate（85∶15,V/V） at flow rate of 0.30 mL/min.The electrospray ionization（ESI source） in positive ion multiple reaction monitoring（MRM） were used for scanning analysis,then,sildenafil and diazepam ion selective channels were： m/z 475.3→58.1 and 285.5→154.0,respectively.RESULTS：The linear range for sildenafil was 1.50-765.90 ng/mL.The lower limit of quantitation was 1.50 ng/mL,and the relative standard deviation of intra-day and inter-day were less than 15%.CONCLUSION： The estalished method is suitable for clinical pharmacokinetic study of sildenafil.

关 键 词：LC-MS/MS 西地那非 内标 

分 类 号：R969.1[医药卫生—药理学]