目的:通过对影响对叶百部碱纯化因素的研究及优化,得到对叶百部碱的最佳纯化工艺。方法:在建立HPLC—ELSD法测定对叶百部碱含量的基础上,采用单因素实验考察不同pH值、萃取溶剂、萃取次数和结晶溶剂对叶百部碱分离纯化的影响,筛选最佳纯化条件。结果:对叶百部药材醇提物酸化离心后,取上清液碱化至pH8左右,以萃取溶剂为石油醚-乙酸乙酯(1:1)为萃取溶剂萃取1次得到总碱浸膏。总碱溶于甲醇中结晶得到纯度大于98%的柱状晶体。结论:本实验得到了一种快速高效获得对叶百部碱的方法。
Objective:To obtain a quick and efficient way to get tuberostemonine by optimizing key factors in this process. Methods : An HPLC - ELSD method was employed to determine the tuberostemonine con- tent in Stemona tuberosa extract. The contents of tuberostemonine were compared under different pH val- ues, extract solvent, extract times and crystalline solvent. Results:The optimal purification conditions were as follows : the acidified ethanol extract was alkalized with ammonia to pH 8, and partitioned with ethyl ac- etate -petroleum ether( 1:1 )for one time to obtain the total alkaloid extract(TAE). The columnar crystals of tuberostemonine could be directly obtained after dissolve the TAE in methanol with the purity more than 98%. Conclusion :A rapid and efficient purification method of tuberostemonine was obtained.