D101大孔树脂对丹酚酸B分离工艺的优化

 目的探讨D101树脂对丹酚酸B分离的最佳工艺。方法丹参提取液经过D101树脂吸附后,以不同乙醇浓度溶液洗脱,采用HPLC测定丹酚酸B的含量。一次正交试验考察丹参提取液浓度、树脂用量、时间等对树脂吸附的影响;二次正交试验考察乙醇浓度、洗脱液用量、流速等对树脂解吸的影响;并绘制丹酚酸B的洗脱曲线。结果树脂用量对丹酚酸B吸附量影响显著,最佳吸附条件为:药材树脂比1:3、色谱柱径高比1:5、药液浓度为原液、上样时间24 h;最佳解吸条件根据考察指标有所不同,以得率为指标时最佳条件为:乙醇浓度70%、洗脱速度2 mL·min^-1、洗脱液用量12倍柱体积;以纯度为指标时最佳条件为:乙醇浓度70%、洗脱速率0.5 mL·min^-1、洗脱液用量8倍柱体积;提高乙醇浓度有利于解吸。结论D101树脂可作为分离丹酚酸B较好分离材料,优化的分离工艺是可行的。

Optimization of Salvianolic Acid B Separation by Macro-reticular Resin D101

OBJECTIVE To research the optimized procedure of salvianolic acid B separation by macro-reticular resin D101.METHODS Dan-shen root extract was absorbed by macro-reticular resin D101,the adsorbed salvianolic acid B was flushed by ethanol aqueous solution and determined by HPLC.The first orthogonal test inspected the effect of extract concentration,resin quantity,time,etc on the adsorption of salvianolic acid B,and the second orthogonal test inspected the effect of ethanol percentage,elution liquid quantity,flow rate on elution.The elution curve was drawn.RESULTS Resin quantity had significant influence on adsorption,the optimum adsorption condition was as follows: raw material vs resin 1∶3,column diameter vs height 1∶5,original concentration,24 h for sampline.The optimized elution condition was different according to yield or purity as index.The optimum conditions for yield were as follows: 70% ethanol,flow rate 2 mL·min^-1,10 times as elution liquid.The optimum condition for purity were as follows: 70% ethanol,flow rate 0.5 mL·min^-1.Eight times as elution liquid Increasing ethanol content was helpful for elution.CONCLUSION D101 resin is better material for the separation of salvianolic acid B,the optimized procedure is practical.