冷却结晶法纯化二氢杨梅素的工艺
Herald of Medicine(2017)
Abstract
目的 建立一种工艺简单,操作方便,适合工业化结晶纯化二氢杨梅素的方法.方法 考察冷却结晶工艺中关键参数如温度、乙醇浓度、活性炭用量、吸附时间等对二氢杨梅素收率、纯度的影响.高效液相色谱法和薄层色谱法验证其纯度,紫外-可见分光光度法测定溶解度与温度和乙醇用量关系,高效液相色谱法测定含量,粉末X射线衍射法和热分析确定晶型.结果 乙醇浓度小于10%,溶剂温度大于85℃,活性炭用量为0.1%~0.3%,吸附时间为1~3 min时,重结晶所得二氢杨梅素收率大于70%,含量大于98%,晶型不变.结论 采用水为溶剂进行结晶纯化,应严格控制温度,温度骤降会导致产率急剧下降,加入10%乙醇即能大幅提高产率,工艺稳健,产率受温度影响较小.
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Key words
Dihydromyricetin,Crystallization,Purification,Process Robustness,Polymorphism
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