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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 screen and purify the macroporous resin suitable for the purification of total flavonoid glycosides in Keqinqidan Recipe. Methods: The ratio of total flavonoid glycosides and calycosin glucoside adsorption capacity, elution rate as an indicator to study D101, AB-8, S-8 type macroporous resin on the active ingredient content, through the single factor test Effect of Concentration of Sample Solution, Sample Amount and Amount of Ethanol on Purification of Total Flavonoid Glycerol Macroporous Resin in Kemin Qidan Prescription. The content of glucoside was determined by HPLC. The detection wavelength was 260 nm. The total flavonoid glycoside content was determined by UV and the detection wavelength was 509 nm. Results: The solution was concentrated to a relative density of about 1.05 (60 ℃), diluted with water to 0.5 g · m L -1, passed through an AB-8 macroporous resin column with an aspect ratio of 1: 6, and washed with 1 BV water The removal rate was 2 BV · h ~ (-1) and the sample volume was 1.5 times of the crude drug solution per 1 g of resin. The eluent flow rate was 4 BV with 70% ethanol 4 BV · h ~ (-1), the eluent was collected. The total flavonoid glycosides and calycosin glucoside transfer rates were 78.22%, 43.81%. Conclusion: The purification process is reasonable and stable, and can be widely used in the large-scale production of Ke Min Qidan Fang.