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超临界CO2萃取-高速逆流色谱分离纯化欧前胡素和异欧前胡素
引用本文:林小静,耿岩玲,刘峰,傅茂润,刘建华,王晓.超临界CO2萃取-高速逆流色谱分离纯化欧前胡素和异欧前胡素[J].山东科学,2011,24(6):39-43.
作者姓名:林小静  耿岩玲  刘峰  傅茂润  刘建华  王晓
作者单位:山东省科学院中药过程控制研究中心,山东省分析测试中心,山东 济南 250014
基金项目:济南市留学人员创业计划,济南市高等院校自主创新计划,山东省科学院科技发展基金项目(科基合字
摘    要:研究了用超临界CO2萃取法从白芷中提取欧前胡素和异欧前胡素,根据正交试验设计确定了超临界萃取最佳工艺条件为温度60 ℃、萃取压力25 MPa和药材粉碎度40~60目,并放大50倍进行萃取试验。利用高速逆流色谱技术分离纯化了欧前胡素和异欧前胡素,溶剂系统为正己烷:乙酸乙酯:甲醇:水(1:0.4:1.1:0.5,V/V)。采用HPLC-DAD,MS对欧前胡素和异欧前胡素进行了定性定量分析,得到产物纯度达99.0%以上,本方法简便快捷,重现性好。

关 键 词:超临界CO2萃取  高速逆流色谱  欧前胡素  异欧前胡素  
收稿时间:2011-05-31

Separation and purification of imperatorin and isoimperatorin with supercritical CO2 fluid extraction- high-speed counter-current chromatography
LIN Xiao-jing,GENG Yah-ling,LIU Feng,FU Mao-run,LIU Jian-hua,WANG Xiao.Separation and purification of imperatorin and isoimperatorin with supercritical CO2 fluid extraction- high-speed counter-current chromatography[J].Shandong Science,2011,24(6):39-43.
Authors:LIN Xiao-jing  GENG Yah-ling  LIU Feng  FU Mao-run  LIU Jian-hua  WANG Xiao
Institution:Process Control Center of Traditional Chinese Medicine, Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan 250014, China
Abstract:This paper addressed the extraction of imperatorin and isoimperatorin from Angelica dahurica (Fisch. ex Hoffm. ) with supercritJcal CO2 extraction method. Orthogonal experiments show that the optimal technological conditions of this extraction method are temperature of 60 ℃, pressure of 2.5 MPa, sample particle size of 40 -60 mesh and 50 times amplification of a preparative supercritical fluid extraction (SFE) system. We separated and purified imperatorin and isoimperatorin with high-speed counter-current chromatography and a two-phase solvent system of 1 : 0.4: 1. 1: 0.5 ( n- hexane-ethyl vs. acetate vs. methanol vs. water, V/V). We also employed HPLC-DAD and MS to perform quantative and qualitive analysis for imperatorin and isoimperatorin. The purities of them were both above 99.0%. The method is convenient and fast,with a high reproducibility.
Keywords:supercritical CO2 fluid extraction  HSCCC  imperatorin  isoimperatorin
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