大孔吸附树脂分离纯化桂花总黄酮工艺研究

Study on the Isolation and Purification Process of Total Flavonoids from Osmanthus fragrans Lour.with Macroporous Absorption Resin

[目的]研究大孔吸附树脂分离纯化桂花总黄酮的工艺条件。[方法]以贵州产桂花为原料,以桂花总黄酮吸附量及回收率等为考察指标,选用AB-8型大孔吸附树脂对桂花总黄酮进行分离纯化,分别采用静态试验和动态试验等考察AB-8型大孔树脂对桂花总黄酮的分离纯化最佳工艺条件及效果。[结果]pH值、洗脱剂、温度、上柱液浓度、径高比、流速、总黄酮与树脂质量比等工艺条件对桂花总黄酮的吸附洗脱量和回收率等影响很大。AB-8型大孔树脂分离纯化桂花总黄酮最佳工艺条件为上柱液pH值4～5;洗脱剂为浓度70%乙醇,料液比为1∶4(g/ml),上柱总黄酮质量与树脂质量比为1∶9.4,上柱液总黄酮浓度为17.86 mg/ml,流速为2～3ml/min;冲洗杂质用水体积2～3 BV,流速为3～4 ml/min;径高比为1.5∶21.6;温度升高,吸附量下降但洗脱率加大。[结论]优选出了大孔吸附树脂分离纯化桂花总黄酮工艺条件,为桂花总黄酮的工业化生产提供试验依据。

[Objective] To study the isolation and purification process of total flavonoids from Osmanthus fragrans Lour.with macroporous Absorption resin.[Method] Taking the adsorption capacity and recovery of total flavonoids as index,the optimum the isolation and purification process of total flavonoids from Guizhou O.fragrans were respectively investigated by static test and dynamic test with AB-8 macroporous Absorption resin.[Result] pH,eluant,temperature,concentration of column-loading sample,diameter-height ratio,current velocity and quality ratio of total flavonoids and Absorption resin had great effects on the adsorption capacity and recovery of total flavonoids from O.fragrans.The optimum conditions for extracting and purifying total flavonoids in static test were： the AB-8 type macroporous resin was blended with 4 times of pH 4-5sample solution（solid-liquid ratio of 1∶4 g/ml） together and then stirred to make it reach the saturation adsorption;then,the isolated resin whose volume was 9.4 times as high as total flavonoids in sample solution was eluted with 70% ethanol.The optimum conditions in dynamic test were： 17.86 mg/ml the extracts of total flavonoids from O.fragrans were loaded into the column with diameter-height ratio of 1.5∶21.6 at a current velocity of 2-3 ml/min and then eluted with 2-3 BV of water to remove impurity at a current velocity of 3-4 ml/min.As the temperature increased,the adsorption capacity declined but the elution rate to enlarge.[Conclusion] The optimum conditions for extracting and purifying total flavonoids with AB-8 type macroporous resin are selected in this study,which could provide experimental basis for the industrial production of total flavonoids from O.fragrans.