银杏叶提取物中银杏内酯B分离纯化工艺研究

Technology of the Separation and Purification of Ginkalide B in Ginkgo Biloba Extract

目的建立一种较为简单的从银杏叶提取物(GBE)中分离纯化银杏内酯B(GB)单体的工艺方法。方法依次通过GBE热水溶解、乙酸乙酯萃取、结晶及重结晶方法对GBE中GB单体进行分离纯化。结果确定GB最佳分离纯化工艺为:将GBE用热水溶解,加入乙酸乙酯萃取3次,合并乙酸乙酯萃取液,萃取液用2%Na HCO3除杂,收集除杂后乙酸乙酯萃取液,减压浓缩至干,用50%乙醇回流溶解后静置析晶,抽滤后得到GB粗结晶,粗结晶用80%甲醇重结晶2次即得,该工艺制备得到的GB单体纯度≥98%,总收率约为60%。结论该工艺稳定、简便易行,适合工业化大生产。

Objective To establish the simple technology of the separation and purifyication of ginkalide B from ginkgo biloba extract.Methods The ginkgo biloba extract was dissolved in hot water, then it was extracted by ethyl acetate, in the end, the ginkgolide B was obtained by crystal and recrystal. Results The best technology of the separation and purification process of GB ginkgo was as follows： the biloba extract was dissolved in hot water, then extracted 3 times by ethyl acetate, extract liquoredulcoration by 2% dicarbonate, the liquorvacuum concen-tration to dry, then the distillate dissolved by 50% ethyl alcohol to crystallize, suction filtration, the coarse crystallization crystallizes and recrystallizes by 80% methyl alcohol. The purity of the ginkgolide B obtained by this methods was equal or greater than 98%, and the yields was about 60%. Conclusion This technology is stabilization and convenience, and is suitable for industrialized production.