天然产物研究与开发 ›› 2015, Vol. 27 ›› Issue (1): 126-133.doi: 10.16333/j.1001-6880.2015.01.026

• 开发研究 • 上一篇    下一篇

土木香内酯与异土木香内酯的提取与纯化工艺

张乐,王梦月,李晓波*   

  1. 上海交通大学药学院中药基因组学实验室,上海 200240
  • 出版日期:2015-01-31 发布日期:2015-02-12

Extraction and Purification of Alantolactone and Isoalantolcatone from Root of Inula helenium

ZHANG Le,WANG Meng-yue, LI Xiao-bo*   

  1. School of Pharmacy,Shanghai Jiao Tong University,Shanghai 200240,China
  • Online:2015-01-31 Published:2015-02-12

摘要: 本文报道了一种从土木香药材中提取以及纯化倍半萜内酯的方法。乙醇回流提取的方法采用正交试验设计方法[L9(34)],考察了4个因素对产率与内酯浓度的影响,最终确定了乙醇回流提取的最佳方法:药材加10倍量的95%乙醇,加热回流提取1次,2 h。而硅胶柱层析的最佳纯化方法为:以100~200目的硅胶,1:3的上样量,径高比为1:2。其洗脱剂成分为石油醚:丙酮(100:3,v/v),洗脱流速为35 mL/min。采用该方法,异土木香内酯与土木香内酯的提取率大于70%,其纯度大于90%。

关键词: 土木香内酯, 异土木香内酯, 正交试验, 硅胶柱层析, 土木香

Abstract: The extraction and purification method of sesquiterpene lactones from the root of Inula helenium L.was optimized.The tests of orthogonal array design [L9 (34)]were performed to analyze the effect of single factors,namely ethanol concentration,extraction duration and times of extraction,on the extraction yield of isoalantolcatone and alantolactone.As the result,the optimal extraction conditions were found as follows:the dried roots of I.helenium were extracted by reflux with 95% ethanol in solid/liquid ratio of 1:10 (w/v) for 2 hrs.The optimized purification process of ethanol extract was achieved by a pressurized silica gel (100-200 mesh) column chromatography with diameter to height ratio of 1:2.The ratio of mixed sample to silica gel was 1:3 (w/w),the eluent composed of petroleum ether (30-60 ℃) and acetone (100:3,v/v),flowed at the rate of 35 mL/min.The extraction yield of the lactones under the optimal method was above 70%,and the purity was above 90%.

Key words: Isoalantolcatone, alantolactone, orthogonal array design, silica gel column chromatography, Inula helenium L.

中图分类号: 

R932