[关键词]
[摘要]
目的 从25-OCH3-原人参二醇(25-OCH3-PPD)非消旋体混合物中分离得到抗肿瘤有效成分20(R)-25-OCH3-PPD (AD-1)。方法 采用结晶法拆分25-OCH3-PPD非消旋体混合物中的AD-1,并对所用溶剂的种类、用量及结晶温度等分离条件进行了优化,探讨溶剂的介电常数和25-OCH3-PPD非消旋体混合物的S/R比例间的关系。结果 25-OCH3-PPD非消旋体混合物(R:59.34%;S:38.35%),在最优条件下,丙酮26 mL、4 ℃时,可以获得AD-1的产率与纯度分别为38.76%、97.83%。结论 溶剂的电解质范围在20.7左右,低饱和度的溶剂以及低温有利于AD-1的分离。
[Key word]
[Abstract]
Objective To separate antitumor constituent AD-1 [20(R)-25-OCH3-protopanoxadiol (PPD)] from non-racemic enatiomeric mixture. Methods A crystallization method has been developed to separate AD-1 from 25-OCH3-PPD non-racemic enatiomeric mixture, the sorts and amount of solvent and crystallization temperature were optimized to obtain the best separative conditions, and the relationship between the S/R percentage of 25-OCH3-PPD non-racemic enantiomeric mixture and dielectric constant of the solvent was discussed. Results Under the optimized conditions (acetone 26 mL, 4 ℃), the yield and purity of AD-1 crystals are 38.76% and 97.83% from 25-OCH3-PPD non-racemic enatiomeric mixture (R: 59.34%; S: 38.35%), respectively. Conclusion The ε values of solvents are about 20.7, and an unsaturated solution and low temperature are beneficial to the separation of AD-1 from 25-OCH3-PPD non-racemic enatiomeric mixture.
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[基金项目]
“十一五”国家重大新药创制项目(2009ZX09102-114);中药标准提取物的工业化色谱制备平台建设(2009ZX09301-012-105B);国家自然科学基金资助项目(81273389)