重楼总皂苷的纯化工艺研究

Studies on purification process of steroidal saponins from Paris polyphylla

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。

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 ob- tained 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： 1 ： 5,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.