干柱层析法制备油茶总皂苷对照品初探

[目的]研究干柱层析法制备油茶皂苷对照品的方法。[方法]原料用60%乙醇超声提取,浓缩至无醇味,石油醚脱酯后用正丁醇按3:1体积比加入萃取。取正丁醇层并真空浓缩至干,干法上样于100目～200目硅胶柱色谱分离,用乙酸乙酯-甲醇-正丁醇-水(2:1:4:7)的上相展层;根据Rf值取出相应的条带并用甲醇淋洗收集蒸干,薄层及理化性质检测。[结果]该方法所制样品由薄层色谱为一点,纯度较高。[结论]该方法简便、实用且制备量大,可作为油茶总皂苷对照品。

Primary Research on Preparation of total oil Tea Saponins as reference Substance by dry column Chromatography

Objective To establish a preparative method for total oil tea saponins as reference substance from the seeds of Camellia Oleiferal Abel.by dry column chromatography. Methods After raw material being extracted with 60 % ethanol, the ethanol extracts were evaporated to alcoholess under reduced pressure. And the solution was extracted by petroleum benzine. Then taking off the upper solution, and adding three times volume of BuOH for extracting, and this time the the upper solution was evaporated to dryness under reduced pressure. The dry powder was fractionated by dry column chromatography on silica gel (100~200 mesh) using the upper solution of EtOAc-MeOH-BuOH-H2O (2:1:4:7) as the eluent. The collected fraction was taken out by the Rf value, And then put the fraction into glass column to collecting the solution by using MeOH as eluent. After that evaporating MeOH with the solution to get the total oil tea-saponins, and decting the saponins by TLC (Thin-layer chromatography )and physical &chemical properties. Results The purity of the product quantitated by TLC was over 98 %. Conclusion The developed method is simple, rapid and the quantity of oil tea saponins also is more than normal preparation methods. All the results show that the praparation substance of all the oil-tea saponins should be as reference substance.