色谱

色谱

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超高效液相色谱-质谱/质谱联用法测定人血浆中的辛伐他汀

王东,秦峰,陈凌云,郝彧,张轶,李发美

  

  1. School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China
  • 收稿日期:2007-09-04 修回日期:2007-10-28 出版日期:2008-05-30 发布日期:1984-03-25
  • 通讯作者: 李发美

Determination of simvastatin in human plasma using ultra-performance liquid chromatography- tandem mass pectrometry

WANG Dong, QIN Feng, CHEN Lingyun, HAO Yu, ZHANG Yi, LI Famei   

  1. School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China
  • Received:2007-09-04 Revised:2007-10-28 Online:2008-05-30 Published:1984-03-25
  • Contact: LI Famei

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摘要：

建立了超高效液相色谱-质谱/质谱联用法(UPLC-MS/MS)测定人血浆中辛伐他汀的浓度。血浆样品经乙醚-正己烷-异丙醇(体积比为80∶20∶3)提取,以洛伐他汀为内标,采用ACQUITY UPLCTM BEH C18柱(50 mm×2.1 mm,1.7 μm)分离,以乙腈-10 mmol/L乙酸铵水溶液(体积比为85∶15)为流动相,流速为0.25 mL/min,通过电喷雾离子化,采用多反应监测(MRM)方式进行正离子检测。线性范围为0.051～20.4 ng/mL,日内及日间测定的相对标准偏差不高于10%,平均回收率为91.6%。方法灵敏度高,分析速度快,操作简便,适用于辛伐他汀药物动力学和生物等效性研究。

关键词: 超高效液相色谱-质谱/质谱联用法, 辛伐他汀, 血药浓度

Abstract:

A rapid, sensitive and specific method has been developed for the determination of simvastatin in human plasma with ultra-performance liquid chromatography-tandem mass spectrometry. Simvastatin and the internal standard （lovastatin） were extracted from human plasma with diethyl ether-n-hexane-isopropanol (80∶20∶3, v/v/v), then separated on a Waters ACQUITY UPLCTM BEH C18 column (50 mm×2.1 mm, 1.7 μm) with isocratic elution at a flow rate of 0.25 mL/min. The mobile phase was composed of 85% acetonitrile and 15% water (containing 10 mmol/L ammonium acetate). Electrospray ionization (ESI) source was applied and operated in positive ion mode. Multiple reaction monitoring (MRM) mode with the transitions of m/z 419.2 →m/z 199.0 and m/z 405.0→m/z 199.0 was used to quantify simvastatin and the internal standard, respectively. The linear calibration curve was obtained in the concentration range of 0.051-20.4 ng/mL. The lower limit of quantification was 0.051 ng/mL. The inter-day and intra-day precision (relative standard deviation) were less than 10%, and the accuracy (relative error) was within -2.7%-0% calculated from quality control samples. The mean extraction recovery of simvastatin was 91.6%. The method was proved to be selective, sensitive, rapid and suitable for the pharmacokinetic study of simvastatin.

Key words: plasma concentration
, simvastatin, ultra-performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）