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采用液相色谱-电喷雾串联质谱法测定人血浆中的赖诺普利含量。

Lisinopril quantification in human plasma by liquid chromatography-electrospray tandem mass spectrometry.

作者信息

Padua Ana A F, Barrientos-Astigarraga Rafael E, Rezende Vinicius M, Mendes Gustavo D, De Nucci Gilberto

机构信息

Department of Pharmacology, State University of Campinas, P.O. Box 6111, Campinas SP, Brazil.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2004 Oct 5;809(2):211-6. doi: 10.1016/j.jchromb.2004.06.021.

Abstract

An analytical method based on liquid chromatography with positive ion electrospray ionization (ESI) coupled to tandem mass spectrometry detection was developed for the determination of Lisinopril in human plasma using Enalaprilat as internal standard. The analyte and internal standard were extracted from the plasma samples by solid-phase extraction using Waters HLB Oasis SPE cartridges and chromatographed on a C8 analytical column. The mobile phase consisted of acetonitrile/water (60:40, v/v) + 20 mM acetic acid + 4.3 mM of triethylamine. The method had a chromatographic total run-time of 6.5 min and was linear within the range 2.00-200 ng/ml. Detection was carried out on a Micromass triple quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM). The precision (CV%) and accuracy, calculated from limit of quantification (LOQ) samples (n = 8), were 8.9 and 98.9%, respectively. The method herein described was employed in a bioequivalence study of two tablet formulations of Lisinopril 20mg.

摘要

建立了一种基于液相色谱-正离子电喷雾电离(ESI)串联质谱检测的分析方法,以依那普利拉为内标物测定人血浆中的赖诺普利。使用Waters HLB Oasis固相萃取小柱从血浆样品中萃取分析物和内标物,并在C8分析柱上进行色谱分离。流动相由乙腈/水(60:40,v/v)+ 20 mM乙酸 + 4.3 mM三乙胺组成。该方法的色谱总运行时间为6.5分钟,在2.00 - 200 ng/ml范围内呈线性。在Micromass三重四极杆串联质谱仪上通过多反应监测(MRM)进行检测。由定量限(LOQ)样品(n = 8)计算得到的精密度(CV%)和准确度分别为8.9%和98.9%。本文所述方法用于两种20mg赖诺普利片剂剂型的生物等效性研究。

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