高纯度京尼平苷的分离纯化

Isolation and purification of geniposide with high purity

以栀子为原料,采用乙醇提取、大孔吸附树脂脱色、乙酸乙酯萃取和丙酮结晶的方法分离纯化京尼平苷。乙醇提取条件:6倍栀子量的质量分数70%乙醇水溶液,于70℃条件下提取2次,每次2 h,京尼平苷的提取率为92.1%。FD802大孔吸附树脂脱色条件:京尼平苷质量浓度为30 mg/mL、栀子黄色素质量浓度为8 mg/mL的提取液,以1 Bv/h的流速通过FD802大孔吸附树脂,栀子黄色素的去除率为91%,京尼平苷的回收率为75%。乙酸乙酯萃取条件:2倍京尼平苷浸膏量的乙酸乙酯,70℃萃取3次,每次0.5 h,京尼平苷总萃取率为≥85%。萃取液浓缩后,进一步采用丙酮结晶的方法,可得纯度85%的京尼平苷,栀子中京尼平苷的总得率≥58%。

The technology of separation and purification about geniposide form the gardenia was established,which using the compositive process of ethanol extraction,macroporous resin bleaching,ethyl acetate extraction and acetone crystallization.The optimum ethanol extraction conditions:ethanol(70 wt%) consumption was six times gardenia's quality,extracting two times under the condition of 70℃,each time for 2 h,and the final extraction rate of geniposide was 92.1%.FD802 macroporous resin bleaching conditions:geniposide concentration of 30 mg/mL,Gardenia yellow pigment concentration of 8 mg/mL,the velocity of flow was one bed volume per hour,and the effect of gardenia yellow pigment's removal rate was 91%,geniposide' recovery rate was 75%.ethyl acetate was two times the effect of geniposide extract,Ethyl acetate extraction conditions:extracting three times under the condition of 70℃,each time for 0.5 h,and the total extraction rate of geniposide was more than 85%.Concentrated liquid extraction,using acetone further crystallization,obtaining in the purity was more than 85%,geniposide and geniposide recovery rate of ≥58%.