鹿茸草中3种苯乙醇苷的分离制备工艺研究

Separation process of three phenolic glycosides from Monochasma savatieri

目的利用大孔吸附树脂以及动态轴向分离技术,建立鹿茸草Monochasma savatieri中3种苯乙醇苷类化合物麦角甾苷(acteoside)、异麦角甾苷(isoacteoside)、torenoside B的最佳分离制备工艺。方法通过静态吸附与解吸附实验和动态分离实验,研究8种常用大孔树脂AB-8、D101、HPD100、LSA-10、LX-11、LX-17、LX-38、XDA-6对该类化合物的分离特性,选出最佳大孔树脂类型;采用所选最佳大孔树脂对3种苯乙醇苷类化合物的纯化工艺参数进行优化。经放大实验得到总苯乙醇苷,再经动态轴向分离得到3种苯乙醇苷类化合物单体。结果优化出的最理想大孔树脂为LX-17;优选的最佳上样质量浓度为原药材1.8 g/m L;最佳吸附时间为150 min;洗脱条件为乙醇-水系统,体积流量为2.5 m L/min,梯度浓度依次为纯水(4 BV)、15%乙醇(4 BV)、60%乙醇(5 BV)以及90%乙醇(2 BV);随后放大10倍进行中试,得到总苯乙醇苷部位,得率为5.25%,其中麦角甾苷15.24%、异麦角甾苷32.14%、torenoside B 29.33%;5 g总苯乙醇苷部位经动态轴向压缩制备柱纯化出3种苯乙醇苷单体成分,分别为麦角甾苷0.127 g,得率2.54%,质量分数为92%;异麦角甾苷0.894 g,得率17.88%,质量分数为95%;torenoside B 0.962 g,得率19.24%,质量分数为98%。结论 LX-17型大孔树脂可作为纯化苯乙醇苷的较佳分离材料,经过优化的分离工艺稳定可靠,有望在工业化生产中推广应用。

Objective The optimal simultaneous separation process of three phenylethanoid glycosides（acteoside, isoacteoside, and torenoside B） from Monochasma savatieri were established using of macrophage resins and dynamic axial column（DAC）. Methods The adsorption/desorption experiments and dynamic separation experiments were performed on eight types of resins（AB-8, D 101, HPD 100, LSA-10, LX-11, LX-17, LX-38, and XDA-6） to find the optimal resin. Then the optimal separation parameters were investigated on the chosen resin. The total phenylethanoid glycosides obtained from the large-scale experiment were further seperated to get acteoside, isoacteoside, and torenoside B, respectively using of DAC system. Results Among these candidate resins, LX-17 was chosen to further obtain the optimal parameters： The optimal feeding concentration of raw materials was 1.8 g/m L; The optimal adsorption time was 150 min; The optimal gradient elute conditions were ethanol/water（0/100, 4 BV; 15/85, 4 BV; 60/40, 5 BV; 90/10, 2 BV）. The large-scale experiments were amplified to 10 folds on the basis of optimal parameters to obtain total phenylethanoid glycosides. Acteoside, isoacteoside, and torenoside B were simultaneously obtained from total phenylethanoid glycosides using DAC system. Conclusion LX-17 and DAC system can be used for the purification of phenylethanoid glycosides, which will have a good future for the application in industry.