摘要
本文以含量为95．59％的天然提取的大黄素粗品为原料，对其纯化工艺进行研究，以获得高纯度大黄素。采用冰醋酸和N，N-二甲基甲酰胺（DMF）作为结晶溶剂，采用交替重结晶的方法对大黄素进行纯化，并就溶剂的用量、溶解温度、析晶温度、以及重结晶溶剂顺序等因素对大黄索纯度的影响进行摸索。优化后的工艺为：先用80倍（mL／g）的冰醋酸重结晶，25℃析晶，再用20倍的DMF重结晶，35℃析晶。HPLC检测结果显示产品含量可达99．60％以上。该方法操作简单，实用性强，为大规模制备高纯度大黄素提供了参考方法。
Conditions of preparing high purity Emodin were studied in this paper. Using 95.59% Emodin extracted from Rheum palmatum L. as raw material, glacial acetic acid and N, N-Dimethylformamide as solvents to recrystallize in sequence. During the optimizing process,five factors including volume of solvent, temperature of dissolving and crystallizing, and the sequence of solvents were studied. As a result, the optimal conditions are obtained, first use 80 folds glacial acetic acid to recrystallize in 25 ℃ ,Then use 20 folds DMF,to recrystallize in the condition of 35 ℃. The purified Emo din was detected by HPLC, and the content was up to 99.60%. The method is convenient and practical,which provides a way to prepare high purity Emedin for industry.
出处
《天然产物研究与开发》
CAS
CSCD
2009年第B10期506-508,共3页
Natural Product Research and Development
基金
科技部科技基础性工作专项重点项目（2007FY130100）
卫生公益性行业科研专项经费（项目编号：200802038）
关键词
大黄素
纯化
交替重结晶
high purity Emodin
preparing
reerystallize in sequence
