LX-70大孔树脂纯化秦艽中龙胆苦苷工艺研究

Study on Purification of Gentiopicroside from Gentiana Macrophylla Pall.by LX-70 Macroporous Resin

目的:筛选适合分离纯化秦艽中龙胆苦苷的大孔树脂并确定纯化工艺参数。方法:以大孔树脂对龙胆苦苷的吸附量和解析率为指标,选择最佳的树脂进行富集。采用单因素实验法对上样浓度、醇洗脱浓度、吸附时间、洗脱体积和流速进行考察,从而确定最佳纯化工艺。结果:LX-70型大孔树脂的吸附和解析效果最佳,其动态饱和吸附量为45.41 mg/g,最佳工艺参数为:龙胆苦苷上样液的质量浓度为30.20 mg/mL,吸附1.5 h,洗脱剂为30%乙醇,乙醇洗脱4B V,洗脱流速1~1.5 BV/h,龙胆苦苷的纯度可达到66.54%,龙胆苦苷的转移率大于95%。结论:LX-70型树脂对龙胆苦苷有较高的吸附量和解析率,洗脱溶剂的用量也更少,其工艺参数可供放大生产参考。

Objective:To screen the suitable macroporous resins for the isolation and purification of gentianoside from Gentiana macrophylla Pall.and to determine the purification process parameters.Methods:The adsorption amount and resolution rate of gentianoside by the macroporous resin were used as indexes to select the best resin for enrichment.The upper sample concentration,alcohol elution concentration,adsorption time,elution volume,and flow rate were examined by a one-way experimental method,to determine the optimal purification process.Results:The LX-70 macroporous resin showed the best adsorption and analysis effect,its dynamic saturation adsorption capacity was 45.41mg/g,and the best process parameters were:the mass concentration of the upper sample solution of gentianoside was 30.20mg/mL,the adsorption was performed for 1.5 h,the eluent was 30%ethanol,the ethanol elution was performed at 4BV,the elution flow rate was 1-1.5BV/h,the purity of gentianaside could reach 66.54%,and the transfer rate of gentianaside was more than 95%.Conclusion:The LX-70 resin has a higher adsorption capacity and resolution rate for gentiopicroside,and the amount of elution solvent is less,and its process parameters can be used as a reference for scale-up production.