粉防己中汉防己甲素的提取分离纯化工艺研究

摘要

目的:建立汉防己甲素的分离纯化工艺.方法:以汉防己甲素得率和纯度为指标,以HPLC法测定产品得率和纯度,采用正交试验设计和单因素试验优选提取纯化工艺.结果:依次采用回流提取、萃取、色谱柱层析、重结晶法可得到纯度较高的汉防己甲素;其中,最佳回流提取工艺为:70%乙醇、料液比1:6、提取时间0.5 h、提取3次;萃取溶剂为氯仿;色谱柱层析填料选择氧化铝.结论:该工艺条件下产品得率达到0.76(g/100 g),纯度达到90%,可用于汉防己甲素的分离纯化.%Objective: To establish the extraction, isolation and purification process of tetrandrine. Methods: The purification process was studied by an orthogonal design and single factor experiments with tetrandrine yield as the index. The product yield and pu-rity were determined by HPLC. Results:The process was conducted with four steps: the reflux extraction, extraction, higher column chromatography and recrystallization to obtain tetrandrine. The optimal conditions of extraction process were as follows: namely 70%ethanol, the solid-liquid ratio of 1 :6(g·ml-1), the extraction time of 0. 5h, extracting three times, the extraction solvent was chloro-form, and alumina column chromatography was the best selection. Conclusion:The process can be used for the separation and purifi-cation of tetrandrine with good yield (0. 76 g/100 g)and high purity(90%).