色谱

色谱

• 研究论文 • 上一篇    下一篇

液相色谱-电喷雾串联质谱法测定人血浆中的艾芬地尔

杨波,陈勇川,向荣凤,杨丹,夏培元,刘松青

  

  1. Department of Pharmacy, Southwest Hospital, Third Military Medical University, Chongqing 400038, China
  • 收稿日期:2007-11-19 修回日期:2008-03-03 出版日期:2008-05-30 发布日期:1984-03-25
  • 通讯作者: 刘松青

Determination of ifenprodil in human plasma using liquid chromatography with electrospray tandem mass pectrometry

YANG Bo, CHEN Yongchuan, XIANG Rongfeng, YANG Dan, XIA Peiyuan, LIU Songqing

  

  1. Department of Pharmacy, Southwest Hospital, Third Military Medical University, Chongqing 400038, China
  • Received:2007-11-19 Revised:2008-03-03 Online:2008-05-30 Published:1984-03-25

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摘要：

建立了测定人血浆中艾芬地尔的液相色谱-串联质谱方法。血浆样品用乙酸乙酯液-液提取后,以甲醇-6 mmol/L乙酸铵溶液(pH 7.40)(体积比为90∶10)为流动相进行分离。在Q TRAPTM串联质谱仪上,以选择性反应离子监测(SRM)方式进行定量分析,用于监测的离子为m/z 326.1→308.2 (艾芬地尔)和m/z 531.0→82.1 (酮康唑,内标)。在6 min内完成了艾芬地尔的检测,工作曲线的线性范围为0.25～50 μg/L,日内、日间精密度分别小于2.7%和6.5%,平均回收率为101.3%～105.0%,检测限为0.08 μg/L。本方法灵敏度高,特异性好,可以用于临床试验的血浆样品的检测。

关键词: 艾芬地尔, 串联质谱, 血浆 , 液相色谱

Abstract:

A method for the determination of ifenprodil levels in human plasma was established. Ifenprodil and the internal standard (IS), ketoconazole, were extracted from the plasma with ethyl acetate using liquid-liquid extraction. The extracts were separated by high performance liquid chromatography (HPLC) using methanol-6 mmol/L ammonium acetate (pH value was adjusted to 7.40) (90∶10, v/v) as the mobile phase, and were then detected using mass spectrometry (MS). Electrospray source was applied and operated in positive ion mode. Selected reaction monitoring (SRM) mode with the transition of m/z 326.1→308.2 was used to quantify ifenprodil, and m/z 531.0→82.1 for IS. The excellent sensitivity and selectivity of the HPLC-MS/MS method allowed quantitation and identification of ifenprodil at low levels with a run time of 6.0 min. The assay was linear over the range from 0.25 to 50 μg/L. The intra-day and inter-day precisions measured as relative standard deviations (RSDs) were less than 2.7% and less than 6.5%, respectively. The average recoveries varied between 101.3% and 105.0%, and the detection limit was 0.08 μg/L. Due to its simplicity and accuracy, the established method is suitable for the application in a pharmaceutical study of the intervenous drop infusion of ifenprodil tartrate.

Key words: ifenprodil, plasma
, tandem mass spectrometry (MS/MS), liquid chromatography (LC)