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目的:建立一种简易的自银杏叶中提取、分离和纯化银杏内酯A的方法。方法:依次通过乙醇溶液搅拌提取、乙酸乙酯萃取、大孔树脂吸附与洗脱及结晶和重结晶对银杏叶中的银杏内酯A进行分离纯化。以银杏内酯A的得率和纯度为指标,对银杏内酯A的分离纯化工艺进行优选。结果:确定银杏内酯A提取、分离和纯化的最佳工艺条件为:将银杏叶乙醇提取物混悬液的酸碱液调节至pH3后进行萃取;选择NM100树脂为固定相,萃取物溶液调节至pH3后上柱,流速控制为1 mL.min-1,再以体积分数为30%和50%的乙醇溶液进行梯度洗脱;收集50%乙醇洗脱液,浓缩后4℃下静置过夜,得粗晶体并进行重结晶,体系中乙醇与水的体积比为2∶1。该工艺制得的银杏内酯A晶体纯度高于99%,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 a simple method of extracting, purifying and purifying ginkgolide A from Ginkgo biloba leaves. Methods: Ginkgolide A in Ginkgo biloba leaves was separated and purified by ethanol extraction, ethyl acetate extraction, macroporous resin adsorption and elution, crystallization and recrystallization. Ginkgolide A yield and purity as an indicator of the ginkgolide A separation and purification process optimization. Results: The optimum conditions for the extraction, separation and purification of ginkgolide A were as follows: the pH value of the solution was adjusted to pH 3 and the extraction was carried out. NM100 resin was used as the stationary phase and the extract solution was adjusted To pH3 after the column, the flow rate control 1mL.min-1, and then the volume fraction of 30% and 50% ethanol gradient elution; collected 50% ethanol eluent concentrated at 4 ℃ overnight The crude crystals were obtained and recrystallized. The volume ratio of ethanol to water in the system was 2: 1. The purity of the ginkgolide A crystal prepared by the process is higher than 99% and the total yield is about 60%. Conclusion: The process is stable, simple and easy, suitable for large-scale industrial production.