化工学报 ›› 2008, Vol. 59 ›› Issue (9): 2283-2288.

• 分离工程 • 上一篇    下一篇

地黄中梓醇的超声提取-树脂分离纯化工艺

樊海燕,杨坤,张晨晓,王先,何宁,王远鹏,孙道华,李清彪   

  1. 厦门大学化学化工学院化学工程与生物工程系,化学生物学福建省重点实验室
  • 出版日期:2008-09-05 发布日期:2008-09-05

Separation and purification of catalpol from Radix Rehmanniae

FAN Haiyan,YANG Kun,ZHANG Chenxiao,WANG Xian,HE Ning,WANG Yuanpeng,SUN Daohua, LI Qingbiao
  

  • Online:2008-09-05 Published:2008-09-05

摘要: 研究了地黄中梓醇的超声提取-树脂分离纯化工艺。结果表明,超声提取的最佳工艺条件为:提取溶剂采用68%(体积)的乙醇,液料体积(ml)质量(g)比5:1,超声时间36 min。考察了10种大孔树脂对地黄粗提液的分离纯化效果,其中以H103对梓醇的纯化效果最佳。通过实验进一步考察了H103的动态吸附性能,得到分离纯化的最佳工艺条件为:上柱液浓度为6.15 mg·ml-1,上柱液流速为1.0 ml·min-1,洗脱剂为75%乙醇,洗脱流速为0.5 ml·min-1,洗脱体积为3.33 BV(bed volume)。提取、纯化两步操作后梓醇纯度达到62.39%。

关键词:

地黄, 梓醇, 超声提取, 大孔树脂

Abstract:

An ultrasonic extraction technology of preparing catalpol from Radix Rehmanniae was optimized by a uniform experimental design.The optimum conditions for ultrasonic extraction were thus established: 68% (vol) ethanol aqueous solution as extraction solvent, the volume(ml) to mass(g) ratio of extraction solvent to feed of 5∶1, the ultrasonic treatment time of 36 min.The crude catalpol obtained from the optimized ultrasonic extraction technology was further purified by selective adsorption with macroporous resin.The adsorption capacities and desorption yields of ten kinds of macroporous resins for catalpol were investigated.The results showed that H103 resin possessed the best performance.The properties of dynamic adsorption and desorption of H103 resin for catalpol were subsequently investigated on adsorption column.The optimum conditions for adsorption and desorption were determined.The concentration of catalpol in the loaded sample solution was 6.15 mg·ml-1, the flow rate was 1.0 ml·min-1, the volumetric percentage of ethanol in the eluting solvent was 75%,the elution flow rate was 0.5 ml·min-1 and the elution volume was 3.33 BV(bed volume).Under the above conditions, the purity of catalpol product eluted from the column packed with H103 resin reached 62.39% while that of the crude catalpol was only 10.01%.

Key words:

地黄, 梓醇, 超声提取, 大孔树脂