知母皂苷BⅡ的提取及大孔树脂纯化工艺研究

Study on the Extraction Process and Macroporous Resin for Purification of Timosaponin BⅡ

目的:优选知母药材中知母皂苷BⅡ的提取纯化工艺。方法:以知母皂苷BⅡ提取率为考察指标,采用L9(34)正交试验,对知母皂苷BⅡ回流提取工艺进行优化;并考察8种大孔树脂对知母皂苷BⅡ的吸附和解析性能,选出最优树脂,确定最佳纯化工艺条件。结果:正交试验表明,知母皂苷BⅡ的最佳提取工艺为:50%乙醇加热回流提取2次,每次2h,溶剂用量分别为8.5倍、6倍、6倍。通过对树脂的考察,优选出对知母皂苷BⅡ吸附率和解析率都很高的HPD100树脂,上样浓度为0.23g/mL,最大上样量为4/5BV,以3BV水和6BV的20%乙醇洗脱杂质后,用5BV的50%乙醇洗脱得到质量分数为50%左右的知母皂苷BⅡ。结论:优选得到的提取工艺稳定可行,适合知母皂苷BⅡ的工业化提取生产。

Objective： To optimize the extraction process and macroporous resin for purification of Timosaponin B Ⅱ from Anemarrhena asphodeloides. Methods ： Orthogonal design L9 （ 3^4 ） was employed to optimize the circumfluence extraction conditions by taking the extraction yield of Timosaponin B Ⅱ as index. The absorption-desorption characteristics of eight kinds of macroporous resins were evaluated, then the best resin was chosen to optimize the purification process conditions. Results： The optimum extraction conditions were as follows ： the herb was extracted for 2 times （2 hours each time） with 8.5-fold 50% ethanol at the first time and 6-fold 50% ethanol at the second time. HPD100 resin showed a good property for the absorption-desorption of Timosaponin B U. The optimum technological conditions of HPD100 resin were as follows：the solution concentration was 0.23 mg/mL, the amount of saturated adsorption at 4/5 body volumn （BV） resin, the HPD100 resin was washed with 3 BV water and 6 BV 20% ethanol solution to remove the impurity,then the Timosaponin B Ⅱ was desorbed by 5 BV ethanol solution. The purity of Timosaponin B Ⅱ was about 50%. Conclusion：The optimized extraction process and purification is stable, efficient and suitable for industrial production.