从白鲜皮中同时制备梣酮、白鲜碱、黄柏酮单体的方法  

The Simultaneous Preparation of Fraxinellone,Dictamine and Obacunone from Dictamnus Dasycarpus. Turcz

作　　者：李翔[1] 张新申[1] 邓赟[2] 蒋小萍[1] 

机构地区：[1]四川大学轻工与食品学院,四川成都610065 [2]成都中医药大学药学院

出　　处：《四川大学学报（工程科学版）》2007年第4期68-72,共5页Journal of Sichuan University (Engineering Science Edition)

基　　金：国家科技部中小企业创新基金资助项目(04C26225100815)

摘　　要：以HPLC测定计算的梣酮、白鲜碱、黄柏酮3种单体的总单体得率为指标,探讨了提取溶媒、提取方式、提取时间、液料比和提取次数对提取效果的影响,并运用正交试验对提取工艺进行优选;提取得到的浸膏进行一次硅胶柱层析和重结晶即分离纯化出3种单体;单体经波谱方法进行结构鉴定,经TLC和HPLC进行纯度检查和含量测定。结果显示,最佳的提取工艺为加入药材重量6倍的乙酸乙酯回流提取3次,每次1 h;分离纯化后的3种单体纯度高,用其作为对照品对白鲜皮药材进行含量测定结果满意。实验表明提取工艺及分离方法能同时制备3种单体,方法简单快速,单体的纯度和回收率高。The effects of extraction solvent, extraction method, extraction time, ratio of solvent to raw material and number of times on the total yield of fraxinellone, dictamine and obacunone were studied, and the extraction condition were optimized by orthogonal experiment. By the method of one time chromatography and recrystallization, three compounds were separated from the residue. The structures of the compounds were elucidated on the basis of spectral analysis, and the purity and concentration was detected by TLC and HPLC. The results showed that the optimum extraction condition was that the raw material was reflux extracted by EtoAc （1 h × 3 times） , with ratio of solvent to raw material 6： 1. These compounds can be used as reference substance for the content determination. The method established can simultaneously separated fraxinellone, dictamine and obacunone from Dictamnus dusycarpus Turcz. , with simple and rapid procedure, high purity and yield of the three compounds.

关 键 词：梣酮 白鲜碱 黄柏酮 白鲜皮 提取 正交试验 

分 类 号：TQ164.2[化学工程—高温制品工业]