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一种用于定量测定大鼠血浆中冬凌草甲素的快速高效液相色谱/电喷雾质谱联用方法。

A rapid HPLC/ESI-MS method for the quantitative determination of oridonin in rat plasma.

作者信息

Xu Wen, Sun Jin, Zhang Tingting, Tang Jingling, Li Haiyan, Fang Jinling, Chen Dawei, He Zhonggui

机构信息

Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, PR China.

出版信息

Pharmazie. 2006 Sep;61(9):757-9.

Abstract

A rapid and accurate method using liquid chromatography with electrospray ionization mass spectrometric detection (HPLC/ESI-MS) was developed and validated for the determination of oridonin in rat plasma. The analytes were extracted with ethyl acetate-n-butyl alcohol (100:2, v/v) after spiking the samples with ethyl hydroxybenzoate (internal standard). The separation was carried out on a Diamon-sil C18 column with an isocratic mobile phase consisting of methanol-water (80:20, v/v) at a flow rate of 1.0 ml/min. The lower limit of quantification (LLOQ) of the method was 10 ng/ml and the linear range was 10-4000 ng/ml. The intra-day and inter-day accuracy and precision of the assay were less than 9%. This method has been applied successfully to a preliminary pharmacokinetic study involving the intravenous administration of oridonin to rats.

摘要

建立了一种采用液相色谱-电喷雾电离质谱检测法(HPLC/ESI-MS)快速准确测定大鼠血浆中冬凌草甲素的方法并进行了验证。样品加入对羟基苯甲酸乙酯(内标)后,用乙酸乙酯-正丁醇(100:2,v/v)萃取分析物。在Diamon-sil C18柱上进行分离,等度流动相为甲醇-水(80:20,v/v),流速为1.0 ml/min。该方法的定量下限(LLOQ)为10 ng/ml,线性范围为10 - 4000 ng/ml。该测定方法的日内和日间准确度及精密度均小于9%。该方法已成功应用于一项涉及对大鼠静脉注射冬凌草甲素的初步药代动力学研究。

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