3种贝母类药材贝母素甲和贝母素乙含量测定方法的优化

Determination Optimization of Peimine and Peiminine in Three Varieties of Fritillaria

目的:优化3种贝母中生物碱贝母素甲和贝母素乙的含量测定方法。方法:采用混合溶液回流提取,调p H,再用乙醚萃取的方法制备供试品溶液。色谱柱:Shim-pack VP-ODS(250 mm×4.6 mm,5μm),流动相:乙腈-0.02%二乙胺溶液(75∶25),流速1.0 ml·min^-1,检测器为Alltech 2000ES ELSD,漂移管温度为93℃,载气流速为2.4 L·min^-1。以对照溶液质量浓度的对数值与相应峰面积的对数值计算回归方程。结果:该方法能有效提取出样品中的生物碱,贝母素甲和贝母素乙分离度良好,在一定范围内,线性关系良好,3种贝母中生物碱加样回收率在95.22%~103.51%之间。结论:该方法简便易行,通用性良好,易于执行,为其他贝母类生物碱的含量测定提供了参考。

Objective： To establish an optimized determinationmethod for the alkaloids peimine and peiminine in three varieties of FritiUaria. Methods： The samples were refluxed in a mixed solution, the pH value of the mixed solution was adjusted, and then the solution was extracted by ether to obtain the test solution. A Shim-pack VP-ODS column （4.6 mm x 250 ram,5 μm） was used, the mobile phase consisted of acetonitrile-0.02% diethylamine （75：25）, and the flow rate was 1.0 ml · min-l. An Alhech 2000ES ELSD detector was used, the drift tube temperature and the flow rate of nitrogen carrier gas in the ELSD was set at 93℃ and 2.4 L · min-l, respectively. The regression equation was calculated between the logarithm values of the reference solution concentration and the correspending peak area. Results： The method could effectively extract the alkaloids from the samples. Peimine and peiminine were well separated by the method, and showed good linearity within the respectively given ranges. The average recovery of the alkaloids in the three varieties of FritiUaria was within the range of 95.22% -103.51%. Conclusion： The method is simple, convenient and universal with easy operation,which provides references for the determination of alkaloids in the other varieties of FritiUaria.