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采用固相萃取法通过液相色谱-电喷雾电离质谱联用技术同时测定大鼠血浆中的贝母素甲和贝母素乙。

Simultaneous determination of peimine and peiminine in rat plasma by LC-ESI-MS employing solid-phase extraction.

作者信息

Wu Xiaodan, Chen Juanjuan, Pan Yuanjiang

机构信息

Center of Analysis and Measurement of Zhejiang University, Hangzhou, Zhejiang Province 310029, People's Republic of China.

出版信息

Biomed Chromatogr. 2010 Aug;24(8):902-7. doi: 10.1002/bmc.1384.

Abstract

A simple and reliable LC-ESI-MS method for the determination of peimine and peiminine in rat plasma was developed for the first time. The method was proven to be specific and sensitive by carrying out validation. The analytes were extracted from rat plasma via solid-phase extraction on Waters Oasis MCX cartridges. Chromatography separation was achieved on a C(18) column using 10 mM ammonium acetate (adjusted to pH 3.0 with glacial acetic acid)-acetonitrile (85:15, v/v) as mobile phase. The linear range was 1-100 ng/mL for peimine and peiminine. Intra- and inter-day precisiond were less than 10%. Accuracies were within 85-115% of their nominal concentrations. The limit of quantification was 1 ng/mL for both analytes. The developed assay was successfully applied to pharmacokinetic study of peimine and peiminine in rats orally administered the alkaloids extracts from Bulbus Fritillariae, demonstrating a possible broader spectrum of applications of this method.

摘要

首次建立了一种简单可靠的液相色谱 - 电喷雾电离质谱法用于测定大鼠血浆中的贝母碱和去氢贝母碱。通过进行方法验证,证明该方法具有特异性和灵敏性。通过在Waters Oasis MCX柱上进行固相萃取从大鼠血浆中提取分析物。在C(18)柱上进行色谱分离,使用10 mM醋酸铵(用冰醋酸调节至pH 3.0)-乙腈(85:15,v/v)作为流动相。贝母碱和去氢贝母碱的线性范围为1 - 100 ng/mL。日内和日间精密度均小于10%。准确度在其标称浓度的85 - 115%范围内。两种分析物的定量限均为1 ng/mL。所建立的测定方法成功应用于大鼠口服川贝母生物碱提取物后贝母碱和去氢贝母碱的药代动力学研究,表明该方法可能具有更广泛的应用范围。

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