莫绪飞,吕惠生,张敏华,杨淼,王国庆

• 1:天津大学石油化工技术开发中心教育部绿色合成与转化重点实验室

摘要(Abstract)：

将超临界流体色谱技术应用于当归挥发油中Z-藁本内酯的提纯。采用ZorBax SB-C18色谱柱(250 mm×9.4 mm I.D.,5μm),分别考察了改性剂、流速、压力、温度对色谱分离过程的影响,确定了较适宜的色谱提纯条件:CO2流速10 g·min-1,柱温313.15 K,柱压14 MPa;在此工艺条件下提纯制备Z-藁本内酯单体,得到的产品纯度为98.5%(wt)。研究了色谱过程的热力学规律,绘制色谱分离过程的van’t Hoff曲线,并由此得到了色谱相转移过程焓变为21.46kJ·mol-1,并比较了Z-藁本内酯与相邻组分从流动相到固定相分配过程中焓变和熵变的差值,在此条件下Z-藁本内酯色谱分离过程为焓控过程。

关键词(KeyWords)： 超临界流体色谱;Z-藁本内酯;分离度;热力学

Abstract:

Keywords:

基金项目(Foundation):

作者(Author): 莫绪飞,吕惠生,张敏华,杨淼,王国庆

参考文献(References)：

• [1]State Pharmacopoeia Commission(国家药典委员会).Chinese Pharmacopoeia(中国药典)[S].Beijing(北京):Chemical IndustryPress(化学工业出版社),2000:30,101,313.
• [2]Lu G H,Chan K,Chan C L,et al.Quantification of Z-ligustilides in the roots of Angelica sinensis and related umbelliferousmedicinal plants by high-performance liquid chromatography and liquid chromatography-mass spectrometry[J].J Chromatogr A,2004,1046(1-2):101-107.
• [3]HUANG Bao-hua(黄宝华),ZHANG Kun(张焜),ZHOU Xiao-hui(周晓辉),et al.The study on purification of Z-ligustilide by SFE(超临界CO2萃取当归中藁本内酯工艺条件研究)[J].Chinese Traditional and Herbal Drugs(中草药),2002,33(6):514-515.
• [4]MIAO Aidong(苗爱东),LIANG Qian-de(梁乾德),LIU Yong(刘勇),et al.The study on purification of Z-ligustilide by SPE-HPLCfrom angelica(SPE-HPLC制备色谱法从当归挥发油中分离纯化Z-藁本内酯)[J].Jorunal of Chinese Medicinal Materials(中药材),2005,28(9):778-779.
• [5]Tao Yi,Hao Zhang,Jing Xie,et al.A new procedure for the preparative separation and isolation of Z-ligustilide from the roots ofAngelica sinensis[J].J Sep Sci,2007,30(12):1973-1978.
• [6]Zhang Dalei,Teng Houlei,Liu Ke,et al.Separation and purification of Z ligustilideand senkyunolide a from ligusticumchuanxionghort.with supercritical fluidExtraction and high-speed counter-current chromatography[J].Separation Science and Technology,2006,41(15):3397-3408.
• [7]HAN Bu-xing(韩布兴).Supercritical Fluid Science and Technology(超临界流体科学与技术)[M].Beijing(北京):ChinaPetrochemical Press(中国石化出版社),2005.
• [8]PANG Fei(庞斐),LüHuisheng(吕惠生),LIU Yan(刘岩),et al.The study on purification of Artemisinin by supercritical fluidchromatography(超临界流体色谱纯化青蒿素的研究)[J].J Chem Eng of Chinese Univ(高校化学工程学报),2010,24(4):569-573.
• [9]Lesellier E,West C.Effects of modifiers in subcritical fluid chromatography on retention with porous graphitic carbon[J].Journalof Chromatography,2005,1087(1):64-76.
• [10]HE Yan(何岩),ZHANG Min-hua(张敏华),DONG Xiu-qin(董秀芹).Molecular dynamics simulation for calculating the diffusioncoefficients of acetone,ethylacetate and cyclohexane at inf'inite dilution solution of supercritical CO2(常用夹带剂在超临界CO2中无限稀释扩散系数的MD计算)[J].J Chem Eng of Chinese Univ(高校化学工程学报),2008,22(1):152-156.
• [11]Lane C S,Larry R.Effect of eluent composition on thermodynamic properties in high-performance liquid chromatography[J].AnalChem,1980,52(13):2009-2013.
• [12]van Quach.Evaluation of Polar-Embedded Reversed-Phase Liquid Chromatography Columns and the Temperature dependence of thePhase Ratio[D].Tallahassee:Florida State University,2009.