克敏芪丹方总黄酮苷的大孔树脂纯化工艺优选  

Optimization of Purification Process of Total Flavonol Glycosides in Kemin Qidan Prescription with Macroporous Resin

作　　者：王协和 夏林丽[1] 贺宝莹[1] 宋英[2] 

机构地区：[1]成都中医药大学,成都610075 [2]成都中医药大学附属医院,成都610072

出　　处：《中国实验方剂学杂志》2016年第14期35-38,共4页Chinese Journal of Experimental Traditional Medical Formulae

摘　　要：目的:筛选适合分离纯化克敏芪丹方中总黄酮苷的大孔吸附树脂并优选其纯化工艺参数。方法:以总黄酮苷和毛蕊异黄酮葡萄糖苷的比吸附量、洗脱率为指标,考察D101,AB-8,S-8型大孔吸附树脂对有效成分含量的影响,通过单因素试验考察上样液浓度、上样量及乙醇用量对克敏芪丹方中总黄酮苷大孔树脂纯化工艺的影响。采用HPLC测定毛蕊异黄酮葡萄糖苷含量,检测波长260 nm;采用UV测定总黄酮苷含量,检测波长509 nm。结果:药液浓缩至相对密度约1.05(60℃),加水稀释至0.5 g·m L^(-1),通过径高比1∶6的AB-8型大孔树脂柱,加1 BV水洗除杂,上样吸附和除杂流速均为2 BV·h^(-1),上样量为每1 g树脂上1.5倍生药量药液;加70%乙醇4 BV洗脱,洗脱流速4 BV·h^(-1),收集洗脱液。总黄酮苷和毛蕊异黄酮葡萄糖苷的转移率分别为78.22%,43.81%。结论:该纯化工艺合理、稳定,可推广于克敏芪丹方的大生产应用。Objective ： To select proper macroporous resin for separation and purification of total flavonol glycosides in Kemin Qidan prescription and to determine purification process parameters. Method： Taking adsorption ratio and elution rate of total flavonol glycosides and calycosin-7-O-β-D-glucoside as indexes, impacts of D101, AB-8 and S-8 maeroporous resin on contents of total flavonol glycosides and calycosin-7-O-β-D-glucoside were investigated, single factor tests were adopted to select the concentration of sample liquid, sample loading quantity and the amount of 70% ethanol. Result： Optimum purification process was that condensing the sample solution to a relative density of 1.05 at 60℃ , then centrifuging; centrifugal fluid was diluted to 0.5 g·mL-1, AB-8 type macroporous resin was washed by 1 BV of water, whose diameter and height ratio was 1：6. The flow velocity of sample loading absorption and edulcoration was 2 BV·h-1 and sample loading quantity was that each gram resin matched with solution containing 1.5 times raw medicinal material. Eventually, eluting with 4 BV of 70% ethanol by flow velocity of 4 BV·h-1 and then collecting eluent. Transfer rates of total flavonol glycosides and calycosin-7-O-β-D-glucoside were 78.22% and 43.81%. Conclusion： This optimized purification process is credible, stable and applicable to mass production of Kemin Qidan prescription.

关 键 词：克敏芪丹方 总黄酮苷 大孔树脂 纯化工艺 毛蕊异黄酮葡萄糖苷 

分 类 号：R283.6[医药卫生—中药学] R284.1[医药卫生—中医学]