Quantitative determination of helicid in rat plasma by liquid chromatography–electrospray ionization mass spectrometry and its application to preliminary pharmacokinetic studies

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• 作者：Yuanwei Jia ; Guangji Wang ; Haitang Xie ; Xiaochang Dai ; Yanhua Wang ; Wei Wang ; Meijuan Xu ; Rui Wang ; Chen Yao
• 关键词：Helicid ; LC– ; ESI-MS ; Pharmacokinetics
• 刊名：Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences
• 出版年：2007
• 出版时间：1 March 2007
• 年：2007
• 卷：847
• 期：2
• 页码：72-77
• 全文大小：522 K

文摘

A sensitive and selective liquid chromatography–electrospray ionization mass spectrometry (LC–ESI-MS) method was developed for the identification and quantification of helicid in rat plasma. The method was based on simple liquid–liquid extraction (LLE). A Kromasil C18 column (150 mm × 2.00 mm, 3.5 μm) was used as the analytical column, while a mixture of acetonitrile and 500 μM ammonium chloride was used as the mobile phase. MS detection was performed using a single quadrupole mass spectrometer in a negative selected ion monitoring (SIM) mode. The deprotonated molecules [M + Cl]⁻ at m/z 319.00 and 363.05 were used to quantify helicid and bergeninum (internal standard, I.S.), respectively. The lower limit of quantification of helicid was 1 ng/ml. The method was linear in the concentration range of 1–1000 ng/ml. The intra-day and inter-day precisions (R.S.D. % ) were within 10.0 % for the analyte. Helicid proved to be stable during all sample storage, preparation and analytical periods. The method was successfully applied to a pharmacokinetic study in rats after intragastric administration of helicid with a dose of 50 mg/kg. Only 50 μl of rat plasma at each sampling time was needed for analysis. The proposed method enables unambiguous identification and quantification for the preliminary pharmacokinetic studies of helicid.