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用于定量测定大鼠血浆中威灵仙苷AR的经过验证的液相色谱-串联质谱法及其在药代动力学研究中的应用。

Validated LC-MS/MS assay for the quantitative determination of clematichinenoside AR in rat plasma and its application to a pharmacokinetic study.

作者信息

Wang Dawei, Li Feng, Li Pei, Zhang Ji, Liu Li, Xu Ping, Zhou Lei, Liu Xiaodong

机构信息

Key Laboratory of Drug Metabolism and Pharmacokinetics, China Pharmaceutical University, Nanjing, People's Republic of China.

出版信息

Biomed Chromatogr. 2012 Oct;26(10):1282-5. doi: 10.1002/bmc.2691. Epub 2012 Feb 16.

DOI:10.1002/bmc.2691
PMID:22344977
Abstract

This study aimed to develop and validate a liquid chromatography tandem mass spectrometry method for measuring clematichinenoside AR in rat plasma. Clematichinenoside AR was extracted by solid-phase extraction and chromatographed on an XTerra MS C(8) column. Pulchinenoside B4 was used as the internal standard. Elution was achieved using an isocratic mobile phase of acetonitrile with 0.1% acetic acid (21:79, v/v) at a flow-rate of 0.2 mL/min. The detection was performed by multiple reaction monitoring mode via a negative electrospray ionization interface. Standard curves were linear, ranging from 2.5 to 500 ng/mL. The intra- and inter-day precision values were <14.0% and the accuracy was within ±13%. Extraction recovery ranged from 93.2 to 93.9%. This proposed method was successfully applied to a pharmacokinetic study on clematichinenoside AR in rats after oral administration.

摘要

本研究旨在建立并验证一种用于测定大鼠血浆中威灵仙新苷AR的液相色谱串联质谱法。威灵仙新苷AR采用固相萃取法提取,并在XTerra MS C(8)柱上进行色谱分离。以紫菀苷B4为内标。采用乙腈与0.1%乙酸(21:79,v/v)组成的等度流动相,流速为0.2 mL/min进行洗脱。通过负电喷雾电离接口,采用多反应监测模式进行检测。标准曲线呈线性,范围为2.5至500 ng/mL。日内和日间精密度值均<14.0%,准确度在±13%以内。提取回收率在93.2%至93.9%之间。该方法成功应用于大鼠口服威灵仙新苷AR后的药代动力学研究。

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