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目的:以槐角粗提物为原料,用酸水解,再利用苷元在水解液中溶解性低而沉淀的方法纯化山奈素,并筛选出最佳工艺参数。方法:对工艺中水解时间、水解温度、料液比、冷却沉淀时间及山奈素结晶工艺参数进行研究。结果:确定了槐角粗提物中山奈素水解沉淀纯化工艺为:水解液为甲醇-水-盐酸(5∶3.5∶1.5)溶液,水解时间3h,水解温度70℃,料液比1 g∶5 mL,水解液最佳冷沉时间为1～2 h,可得55%粗晶体,甲醇溶解重结晶可得95%山奈素黄色晶体。结论:通过该工艺可从含12%～14%山奈素的槐角黄酮粗提物中分离纯化得到95%山奈素纯品,可为山奈素的工业化生产提供参考。
OBJECTIVE: Purification of kaempferol with crude extract of Huaijiao, acid hydrolysis, and then using aglycones with low solubility in the hydrolyzate and precipitation, and screening the best process parameters. Methods: The process parameters of hydrolysis time, hydrolysis temperature, solid-liquid ratio, cooling-precipitation time and kaempferol crystallization were studied. Results: The purification process of the crude naivain from Huaijiao was confirmed as follows: the solution was methanol-water-hydrochloric acid (5: 3.5: 1.5), the hydrolysis time was 3h, the hydrolysis temperature was 70 ℃, 5 mL, the best cooling time of the hydrolyzate is 1 ~ 2 h, 55% crude crystals can be obtained, and 95% kaempferide yellow crystals can be obtained by recrystallization from methanol. Conclusion: The purified 95% kaempferol can be isolated and purified from the crude extracts of kaempferol containing 12% ~ 14% kaempferol by this process, which can provide a reference for industrial production of kaempferol.