丹参中丹参酮ⅡA的提取分离研究

Study on the extraction and purification of tanshinon ⅡA from Salvia miltiorrhiza Bge.

目的研究丹参中丹参酮ⅡA的提取纯化工艺。方法以HPLC法为检测手段,对丹参酮ⅡA的提取工艺,D101型大孔树脂分离纯化丹参酮ⅡA的树脂柱径高比、药液质量浓度、上柱吸附体积流量、洗脱体积流量、生药吸附量、解吸溶媒及其最佳用量等因素进行考察。结果丹参中丹参酮ⅡA的最佳提取分离工艺为:避光条件下,丹参药材用6倍量(g·mL-1)的95%(体积分数)乙醇搅拌提取4 h,回收乙醇后用无水乙醇:石油醚(体积比15:85)萃取3次,旋转蒸发除去萃取溶剂,所得浸膏用与药材量比值为1:1(g·mL-1)的60%(体积分数)乙醇溶解上柱,依次用27 BV 68%(体积分数)乙醇洗去杂质,8BV 80%(体积分数)乙醇洗脱,丹参酮ⅡA富集在80%(体积分数)乙醇洗脱部分。结论建立了丹参酮ⅡA的最佳提取纯化工艺,所得浸膏中丹参酮ⅡA质量分数为53.65%。

Objective To establish the optimum process for purifying tanshinon ⅡA from Salvia miltiorrhiza Bge. Methods HPLC was employed to determine tanshinon ⅡA, and the diameter-length ratio of the column with the macroporous resin D101 ,the concentrations of the column-loading solutions, adsorbing volume, eluting volume, adsorptive capacity of crude drugs, desorbing solvents and the optimal amounts were investigated to obtain the optimum process of purification on macroporous resin. Results The optimum process of extraction and purification were as follows：in darkroom, Salvia miltiorrhiza Bge. was extracted through 95% ethanol for 4 h,and the product was condensed and extracted with ethanol and ether（ 15： 85） for 3times, then condensed again and purified through macroporous resin, adsorbing with lg herb in 1 mL 60% ethanol,then eluting with 68% ethanol of 27 BV and 80% ethanol of 8 BV respectively. Tanshinon ⅡA was enriched in the elution of 80% ethanol. Conclusion This method could be used to purify tanshinon Ⅱ A from Salvia miltiorrhiza Bge. The content of tanshinone Ⅱ A was 53.65%.