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采用液相色谱-电喷雾串联质谱法(LC-ESI-MS/MS)对给予五仁醇(五味子提取物)制剂后大鼠血浆中的五味子醇甲和五味子乙素进行高灵敏度测定。

Highly sensitive determination of Schisandrin and Schisandrin B in plasma of rats after administration of Wurenchun (Fructus Schisandrae Chinensis Extracts) preparations by LC-ESI-MS/MS.

作者信息

Tang Jingling, Shao Bing, Liu Yan, Liu Hongmei, Ji Hongyu, Zhu Daling, Wu Linhua

机构信息

Department of Pharmaceutics, School of Pharmacy, Harbin Medical University, Harbin, 150086, China.

出版信息

Biomed Chromatogr. 2010 Jun;24(6):675-81. doi: 10.1002/bmc.1344.

Abstract

A sensitive and specific method based on liquid chromatography-tandem mass spectrometry using electrospray ionization (LC-ESI-MS/MS) has been developed for the determination of Schisandrin and Schisandrin B in rat plasma. A 100 microL plasma sample was extracted by methyl tert-butyl ether after spiking the samples with nimodipine (internal standard) and performed on an XTerra(R)MS-C(18) column (150 mm x 2.1 mm, 3.5 mum) with the mobile phase of acetonitrile-water-formic acid (80:20:0.2, v/v) at a flow rate of 0.2 mL/min in a run time of 8.5 min. The lower limit of quantification of the method was 40 ng/mL for Schisandrin and 20 ng/mL for Schisandrin B. The method showed reproducibility with intra-day and inter-day precision of less than 13.8% RSD, as well as accuracy, with inter- and intra-assay accuracies between 93.5 and 107.2%. Finally, the LC-ESI-MS/MS method was successfully applied to study the pharmacokinetics of Schisandrin and Schisandrin B in rats after administration of Wurenchun commercial formulations to rats.

摘要

已开发出一种基于液相色谱 - 串联质谱联用(LC - ESI - MS/MS)的灵敏且特异的方法,用于测定大鼠血浆中的五味子醇甲和五味子醇乙。将尼莫地平(内标)加入100微升血浆样品后,用甲基叔丁基醚进行萃取,然后在XTerra(R)MS - C(18)柱(150毫米×2.1毫米,3.5微米)上进行分析,流动相为乙腈 - 水 - 甲酸(80:20:0.2,v/v),流速为0.2毫升/分钟,运行时间为8.5分钟。该方法对五味子醇甲的定量下限为40纳克/毫升,对五味子醇乙为20纳克/毫升。该方法具有日内和日间精密度,相对标准偏差(RSD)均小于13.8%,具有重现性,同时具有准确性,批内和批间准确度在93.5%至107.2%之间。最后,LC - ESI - MS/MS方法成功应用于研究大鼠口服五仁醇商业制剂后五味子醇甲和五味子醇乙的药代动力学。

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