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液质联用法测定大鼠血浆中五味子醇甲、五味子甲素血药浓度
Development and Validation of a HPLC-MS/MS Method for Determination of Schisandrin and Deoxyschisandrin in Rat Plasma
【摘要】 目的建立高效液相色谱-质谱联用法测定大鼠血浆中五味子醇甲、五味子甲素血药浓度。方法以地西泮为内标,血浆样品经乙酸乙酯-正己烷萃取后进样,HPLC-MS/MS法分析。采用Eclipse Plus C18(2.1×50mm,3.5μm)色谱柱,流动相为10m M乙酸铵-甲醇,梯度洗脱,电喷雾离子源(ESI),以多反应监测方式(MRM)进行正离子监测。结果五味子醇甲、五味子甲素在检测范围内具有良好的线性关系。测定方法的精密度、准确度、基质效应、稳定性良好,符合规范要求。结论该方法操作简便、灵敏、准确、快速,适用于五味子醇甲、五味子甲素的进一步研究。
【Abstract】 OBJECTIVE To develop an HPLC-MS/MS method for determination of schisandrin and deoxyschisandrin in rat plasma. METHODS Diazepam was used as internal standard. Plasma was extracted with ethyl acetate and samples were separated on an Eclipse Plus C18 column(2. 1 × 50 mm,3. 5μm) with gradient elution using a mobile phase that consisted of 10 m M ammonium acetate-methanol. The eletrospray ion-ization(ESI) with positive source of the mass spectrometer and detected in multiple reaction monitor(MRM) mode. RESULTS The calibration curve of Schisandrin and Deoxyschisandrin showed a good linear relation-ship in the detection range. The method had good precision,Accuracy,matrix effects,methods of recovery and stability met the analysis requirements. CONCLUSION This established method is sensitive,simple,rapid,and stable and applicable to the analysis of deoxyschisandrin and schisandrin for its further study.
【Key words】 Schisandrin; Deoxyschisandrin; Schisandrin B; Rat; Plasma concentration of drug; LC-MS/MS;
- 【文献出处】 海峡药学 ,Strait Pharmaceutical Journal , 编辑部邮箱 ,2018年07期
- 【分类号】R285.5
- 【下载频次】221