大孔树脂对龙须藤中4种多甲氧基黄酮类化合物的纯化研究

目的 优选分离纯化龙须藤中4种多甲氧基黄酮的大孔吸附树脂及相应的工艺条件.方法 采用HPLC法测定5,6,7,5'-四甲氧基-3',4'-亚甲二氧基黄酮(PMF1)、5,6,7,3',4',5'-六甲氧基黄酮(PMF2)、5,6,7,3',4'-五甲氧基黄酮(PMF3)和5,7,3',4',5'-五甲氧基黄酮(PMF4)的质量分数,考察树脂类型、上样吸附速率、乙醇体积分数、洗脱剂用量等参数,优选出最佳的大孔吸附树脂纯化工艺.结果 NKA型大孔树脂用于分离纯化龙须藤中4种多甲氧基黄酮的效果较好,其最佳纯化工艺参数为:上样液生药浓度0.66 g/mL,吸附速率为2 BV/h,以5 BV蒸馏水和8 BV的35%乙醇洗脱杂质,然后用75%乙醇10 BV洗脱.收集75%乙醇洗脱液,烘干,所得固体样品中4种多甲氧基黄酮的总质量分数为35.98%.结论 NKA型大孔树脂可用于龙须藤中多甲氧基黄酮的富集,优选得到的纯化工艺稳定可行.

Optimization of separation and enrichment process of four polymethoxyflavones from Bauhinia championii (Benth.) Benth by macroporous resin

Objective To optimize adsorption function of macroporous resins for the separation and purification of four polymethoxyflavones from Bauhinia championii (Benth.) Benth.Methods HPLC was adopted to determine 5,6,7,3'-tetramethoxy-4',5'-methylenedioxyflavone (PMF1),5,6,7,3',4',5'-hexamethoxyflavone (PMF2),5,6,7,3',4'-pentamethoxyflavone (PMF3),and 5,7,3',4',5'-Pentamethoxyflavone (PMF4).The best purification process was selected by the parameters such as resin type,sample adsorption rate,ethanol volume fraction,and the amount of the elution agent and so on.Results It showed a good purifying profile on NKA resin with the conditions as follows: the concentration of sample extract was 0.66 g/mL,the flow rate was 2 BV/h,then eluting successively with 5 BV water and 8 BV 35% ethanol solution to remove impurities,elution with 75% ethanol at length.75% ethanol eluate was collected and dried,and the total mass fraction of four polymethoxyflavones in the solid sample was 35.98%.Conclusion NKA-type macroporous resin could be used for the enrichment of polymethoxyflavone in B.championii,and the purification process is stable and feasible.