摘要:
目的:优选重楼总皂苷的纯化工艺。方法:综合运用醇溶液调节pH、醇提和大孔吸附树脂技术,以总皂苷含量、总皂苷收率为指标,优选重楼总皂苷的纯化工艺。结果:优化后的重楼总皂苷的纯化工艺条件为:70%乙醇提取液调节pH值至9,抽滤,将滤液调pH值至中性,浓缩至0.5 g生药/mL,调pH值至8,离心(4000 r/min,30 min),上清液部分上D101大孔树脂柱纯化(上样量为70%饱和吸附量,径高比为1:5,上样流速为4.5 BV/h,纯化溶剂为20%乙醇,用量为6 BV,洗脱溶剂为70%乙醇,用量为8 BV,流速为7 BV/h)。采用本工艺制备的中间体中总皂苷含量达71.6%,总皂苷收率为85.71%。结论:验证试验结果表明,优选出的工艺稳定、合理、可行。
Abstract:
Objective :To optimize the purification process of saponins from Paris polyphylla Smith. Methods :According to the purity and gaining rate of total saponins,the optimum purifying process was obtained by a combination of adjusted the pH in alcohol solution,alcohol extracting-water precipitating and macroporous resin techniques. Results :The optimum purification conditions were obtained as follows:70% alcohol solution,the pH of which was adjusted to 9,was suckingly filtrated.After the pH to 7,the filtrate was concentrated to 0.5 g/mL and then centrifuged(4 000 r/min,30 min).The clear supernatant liquid was purified by D101 macroporous resin(loading sample volume:70% adsorption capacity,column diameter vs height:15,loading flow rate:4.5 BV/h,purification solvent:20% alcohol,volume:6 BV,eluting solvent:70% alcohol,volume:8 BV,eluting flow rate:8 BV/h).The purity and gaining rate of total saponins prepared by the optimum process were 71.6% and 85.71% respectively. Conclusion :The purification process of saponins obtained by this experiment is steady,reasonable and feasible.
点击查看大图
下载:
