丹参中丹参酮ⅡA和丹酚酸B的提取与纯化工艺研究

Extraction and Purification of Tanshinone ⅡA and Salvianolic Acid B from Salvia Miltiorrhiza Bunge

建立了同时提取丹参中丹参酮ⅡA与丹酚酸B两种主要活性成分的方法及丹酚酸B的纯化工艺。以丹参酮ⅡA与丹酚酸B的含量为评价指标,采用正交实验优化提取工艺,所得最优提取工艺为:用8倍量70%乙醇回流提取3次,每次1 h。丹参酮ⅡA的提取率在90%以上,丹酚酸B的提取率在80%以上。提取物浸膏用热水溶解,过滤,滤液浓缩为1 m L含约0.5 g生药的溶液,取150 m L以2 BV/h的速度上D101大孔树脂柱;然后用6 BV的水洗脱,再以4 BV/h的流速用8 BV的30%乙醇洗脱除杂,以2 BV/h的流速10 BV60%乙醇富集,得到纯度大于75%丹酚酸B,验证实验表明该工艺稳定可行;最后经过洗涤和甲醇重结晶,得到纯度大于99%的丹酚酸B,总得率为2.86%(以干燥根茎计算)。

A method for simultaneous extraction of tanshinone ⅡA and salvianolic acid B from the Salviamiltiorrhiza Bunge and the purification of salvianolic acid B was developed. The extraction process was optimized by orthogonal design with the content of tanshinone ⅡA and slvianolic acid B as evaluation indexes. The optimal extraction process was as follows: S. miltiorrhizapowder was extracted by 8 times of 70% ethanol with at 85 ℃( reflux) for three times in 1 h. The extraction rate of tanshinone ⅡA was higher than 90%,and the extraction rate of salvianolic acid B was higher than80%. The extract was dissolved in hot waterand filtered,the filtrate was concentrated to 1 m L of a solution containing about 0. 5 g of crude drugwith the volume of 100 m L was loaded on the D101 macroporous resin column with the sample flow rate of 2 BV/h,and then column was washed by 6 BV of water,8 BV of 30% ethanol with the flow rate of 4 BV/h for removing impurities,10 BV of 60% ethanol with 2 BV/h flow rate for purifying,to obtain more than 75% purity of salvianolic acid B,verification experiments showed that the process was stable and feasible; Finally,after washing and methanol recrystallization,more than 99% purity salvianolic acid B was obtained,the total yield of about 2. 86%( based onthe dried rhizomes).