大孔吸附树脂分离纯化淫羊藿EF5黄酮

Separation and purification EF5 flavonoids of epimedium by macroreticular resin

目的:采用HPLC法和UV法监测AB-8大孔吸附树脂分离纯化以淫羊藿苷、朝藿定A、朝藿定B、朝藿定C和宝藿苷I这五种黄酮为主要成分的淫羊藿EF5黄酮并筛选出最佳分离纯化工艺参数。方法:采用UV法,以淫羊藿总黄酮洗脱率为指标,考察树脂对淫羊藿总黄酮的吸附容量、解吸附率、吸附动力学,以确定树脂分离纯化淫羊藿EF5黄酮的最佳吸附性能;采用HPLC法,以淫羊藿EF5黄酮中五种黄酮单体的洗脱率为指标,考察洗脱液浓度和洗脱液用量等参数,确定淫羊藿EF5黄酮的最佳洗脱参数。结果:AB-8大孔吸附树脂对淫羊藿总黄酮的吸附容量以湿树脂计为(58.37±2.36)mg·g-1,解吸附率为(86.77±2.32)%,最佳吸附时间为180min,最佳洗脱液为60%乙醇,最佳洗脱液用量为5BV,纯化后真空干燥所得棕褐色淫羊藿EF5黄酮粉末中朝藿定A、朝藿定B、朝藿定C、淫羊藿苷和宝藿苷I的含量分别为3.51%、4.87%、1.22%、33.05%、1.36%,淫羊藿EF5黄酮纯度为44%。结论:AB-8大孔吸附树脂分离纯化得到的淫羊藿EF5黄酮的纯度较高,适合工业生产。

Objective： To select the best purification process parameters,epimedium EF5 flavonoids which mainly contain epimendin A,epimendin B,epimendin C,icariin,and baohuoside I were separated and purified with AB-8 macroreticular resin and the processes were monitored by HPLC and UV. Method： Taking the elution rate of epimedium total flavonoids as index,adsorption capacity,desorption rate and adsorption kinetics of epimedium total flavonoids were studied to determine the best adsorption properties of the separation and purification of epimedium EF5 flavonoids by resin. Meanwhile,taking the elution rate of five flavonoids as index,the concentration and usage amount of eluent were studied to determine the optimal elution parameters of separation and purification of epimedium total flavonoids by AB-8 macroporous resin. Result： To calculate by wet resin,its adsorption capacity was（58.37±2.36）mg·g-1.The desorption rate of epimedium total flavonoids was（86.77±2.32）%,the optimal adsorption time was 180 min,the best eluent was60% ethanol,the best usage amount of eluent was 5 BV. After vacuum drying epimedium EF5 flavonoids were purified,the purity of epimendin A,epimendin B,epimendin C,icariin,and baohuoside I were 3.51% 、4.87% 、1.22% 、33.05% 、1.36%,respectively. The purity of epimedium EF5 flavonoids was 44%. Conclusion： The high purity of epimedium EF5 flavonoids can be achieved by AB 8-macroporous resin,and it is suitable for industrialized production.