LC-MS/MS内标法测定人血浆中西地那非的浓度

中国临床药理学与治疗学 ›› 2011, Vol. 16 ›› Issue (11): 1272-1276.

LC-MS/MS内标法测定人血浆中西地那非的浓度

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

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, 长沙 410078,湖南;
²中南大学药学院,长沙 410078,湖南

收稿日期:2011-08-31 修回日期:2011-10-20 出版日期:2011-11-26 发布日期:2011-11-29
通讯作者: 欧阳冬生,男,博士,副教授,硕士生导师,研究方向:遗传药理学与临床药代动力学。Tel: 13307313736 E-mail: ouyangyj@163.com
作者简介:邓晓兰,女,硕士研究生,研究方向:临床药理学。Tel: 13755116722 E-mail: dxl1220@163.com

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

DENG Xiao-lan¹, TAN Zhi-rong¹, CHEN Yao¹, LI Hui¹, WANG Yi-cheng¹, HUANG Qi², OUYANG Dong-sheng¹

¹Institute of Clinical Pharmacology, Hunan Key Laboratory of Pharmacogenetics,Central South University , Changsha 410078 , Hunan, China;
²School of Pharmaceutical Sciences, Central South University , Changsha 410078 , Hunan,China

Received:2011-08-31 Revised:2011-10-20 Online:2011-11-26 Published:2011-11-29

摘要/Abstract

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 XTerra MS C₁₈ (150 mm×2.1 mm, 5 μm)柱分离,流动相为甲醇 : 10 mmol/L 醋酸铵=85∶15(V/V),流速为 0.30 mL/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/z 475.3→58.1 和 285.5→154.0。结果: 西地那非的线性范围为 1.50~765.90 ng/mL,最低检测浓度为 1.50 ng/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。

关键词: LC-MS/MS, 西地那非, 内标

Abstract: 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.

Key words: LC-MS/MS, Sildenafil, Internal standard

中图分类号:

R969.1

邓晓兰, 谭志荣, 陈尧, 李慧, 王医成, 黄琪, 欧阳冬生. LC-MS/MS内标法测定人血浆中西地那非的浓度[J]. 中国临床药理学与治疗学, 2011, 16(11): 1272-1276.

DENG Xiao-lan, TAN Zhi-rong, CHEN Yao, LI Hui, WANG Yi-cheng, HUANG Qi, OUYANG Dong-sheng. Determination of sidenafil concentration in human plasma by LC-MS/MS with internal standard method[J]. Chinese Journal of Clinical Pharmacology and Therapeutics, 2011, 16(11): 1272-1276.

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