大孔吸附树脂联用硅胶柱层析法分离纯化冬凌草甲素

Separation and Purification of Oridonin by Macro-porous Resin and Silica Column Chromatography

目的:建立大孔吸附树脂联用硅胶柱层析法分离纯化冬凌草甲素的工艺流程。方法:将冬凌草粉碎,用95%乙醇提取,浓缩成浸膏;以冬凌草甲素含量为指标,采用大孔吸附树脂联用硅胶柱层析法分离纯化冬凌草甲素,并用红外光谱、熔点测定和高效液相色谱(HPLC)法对重结晶产品的纯度和结构进行分析和表征。结果:优化的工艺为采用苯乙烯型大孔吸附树脂(HZ-841)先对浸膏进行粗分离,再选取乙酸乙酯-石油醚(6:4,V/V)为洗脱溶剂,石油醚-丙酮(2:3,V/V)为重结晶溶剂进行硅胶柱分离纯化,在此条件下,得到的冬凌草甲素含量为96.11%,提取率达到0.86‰。结论:所选工艺简单、可行,使用溶剂安全、无毒,提取效率高,可用于分离纯化冬凌草甲素。

OBJECTIVE：To establish macro-porous resin and silica column chromatography for the separation and purification of oridonin.METHODS：Rabdosia rubescens was shattered and extracted with 95% ethanol,then concentrated to extract.Taking the content of oridonin as index,the oridonin was separated and purified by macro-porous resin and silica column chromatography.The structure and purity of the recrystallized products were analyzed and characterized with IR spectra,smelting point and HPLC.RESULTS：The optimal technology was as follows：polystyrene-type macroporous absorbing resins（HZ-841）was used to separate extract roughly and silica column was used for purification with acetic ether-petroleum benzin（6：4,V/V）as elution solvent and petroleum benzin-acetone（2：3,V/V）.Under this condition,the content of oridonin was 96.11% and the extraction ratio reached to 0.86‰.CONCLUSIONS：The technology is simple and feasible,and solvents used are safe and non-toxic with high extraction efficient.It can be used for the separation and purification of oridonin.