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超高效液相色谱-电喷雾电离质谱法测定人血浆中喹那普利和喹那普利拉

Determination of quinapril and quinaprilat in human plasma by ultraperformance liquid chromatography-electrospray ionization mass spectrometry.

作者信息

Dasandi Bhavesh, Shah Sanjay

机构信息

Department of Chemistry, Pilvai Science college, Pilvai, Vijapur, Gujarat State, India.

出版信息

Biomed Chromatogr. 2009 May;23(5):492-8. doi: 10.1002/bmc.1143.

DOI:10.1002/bmc.1143
PMID:19016233
Abstract

A novel, specific and sensitive ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of quinapril and its active metabolite quinaprilat in human plasma. The method involves a simple, one-step extraction procedure coupled with an Acquity UPLC BEH C(18 )column (100 x 2.1 mm, i.d., 1.7 microm) with isocratic elution at a flow-rate of 0.2 mL/min and lisinopril as the internal standard. Detection was performed on a triple-quadrupole tandem mass spectrometer in multiple reaction monitoring mode via electrospray ionization. Using 250 microL plasma, the methods were validated over the concentration range 5.010-500.374 ng/mL for quinapril and 10.012-1000 ng/mL for quinaprilat, with a lower limit of quantification of 5.010 ng/mL for quinapril and 10.012 ng/mL for quinaprilat. The intra- and inter-day precision and accuracy were within 10.0%. The recovery was 85.8, 62.6 and 61.3% for quinapril, quinaprilat and lisinopril, respectively. Total run time was 3.0 min only.

摘要

建立了一种新颖、特异且灵敏的超高效液相色谱串联质谱法(UPLC-MS/MS),用于同时测定人血浆中喹那普利及其活性代谢物喹那普利拉。该方法包括一个简单的一步萃取程序,结合Acquity UPLC BEH C(18) 柱(100×2.1 mm,内径,1.7微米),以0.2 mL/min的流速等度洗脱,以赖诺普利作为内标。在三重四极杆串联质谱仪上通过电喷雾电离在多反应监测模式下进行检测。使用250微升血浆,该方法在喹那普利浓度范围为5.010 - 500.374 ng/mL和喹那普利拉浓度范围为10.012 - 1000 ng/mL内进行了验证,喹那普利的定量下限为5.010 ng/mL,喹那普利拉的定量下限为10.012 ng/mL。日内和日间精密度及准确度均在10.0%以内。喹那普利、喹那普利拉和赖诺普利的回收率分别为85.8%、62.6%和61.3%。总运行时间仅为3.0分钟。

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