医药导报2017，Vol.36Issue(8)：912-917,6.DOI:10.3870/j.issn.1004-0781.2017.08.017
冷却结晶法纯化二氢杨梅素的工艺
Process of Purification of Dihydromyricetin by Cooling Crystallization
摘要
Abstract
Objective To development a cooling crystallization process that is suitable for industrial preparation of purified dihydromyricetin.Methods Screen design was used to investigate effects of process parameters such as,temperature,concentration ethanol aqueous,quantity of activated charcoal and adsorption time on yield and purity of dihydromyricetin.Purity was verified by high performance liquid chromatography and thin layer chromatography.The solubility of dihydromyricetin in water at viable temperature and ethanol proportion was also determined by UV spectrophotometry.The solid form was characterized by thermal analysis and powder X-ray diffractometry.Results When temperature was ＞ 85 ℃,ethanol concentration ＜ 10％,dosage of activated charcoal 0.1％-0.3％,and adsorption time 1-3 min,yield of dihydromyricetin was more than 70％,and the purity greater than 98％.The crystals,prepared by cooling crystallization from water and ethanol aqueous,had the same physical form and crystal habit.Conclusion Cooling crystallization from low concentration of ethanol aqueous gets higher yield and the process is more robust than crystallization from water.关键词
二氢杨梅素/结晶/纯化/工艺稳健性/晶型Key words
Dihydromyricetin/Crystallization/Purification/Process Robustness/Polymorphism分类
医药卫生引用本文复制引用
谢雪佳,王晨光,侯小龙,熊微,王文清..冷却结晶法纯化二氢杨梅素的工艺[J].医药导报,2017,36(8):912-917,6.基金项目
国家自然科学基金资助项目(81503013) （81503013）
