离线二维反相液相色谱/超临界流体色谱在瓜蒌子分离中的应用  

Application of off-line two dimensional reversed-phase liquid chromatography/supercritical fluid chromatography to the separation of the seeds of Trichosanthes kirilowii Maxim.

作　　者：袁云[1] 辛华夏 彭子悦 傅青[1] 金郁[1] 

机构地区：[1]华东理工大学药学院,上海200237

出　　处：《色谱》2017年第7期683-687,共5页Chinese Journal of Chromatography

基　　金：国家自然科学基金(21305138)~~

摘　　要：发展了离线二维反相液相色谱/超临界流体色谱(2D RPLC/SFC)分离瓜蒌子的方法。实验在第一维采用反相色谱,按色谱峰收集从瓜蒌子样品中制备得到的12个组分(F_1~F_(12)),并将得到的组分在第二维使用SFC分离。这些组分在RPLC和SFC的分离对比说明,该二维方法具有良好的分离正交性,可至少检测到150个色谱峰,对于解决结构相似物质的分离、微量成分的富集表现出了明显的优势。SFC方法采用了乙醇-正己烷(3∶7,v/v)的混合溶剂作为改性剂,既提供了适当的洗脱能力,也保证了在上样量增加时满足样品溶解的要求。此二维分离体系可放大到制备水平用于化合物的制备,为瓜蒌子化学成分的纯化制备提供技术支持,为其物质基础研究提供参考。An off-line two dimensional reversed-phase liquid chromatography/supercritical fluid chromatography （2D RPLQ/SFC） method was developed for the separation of the seeds of Tri-chosanthes kirilowii Maxim. （T. kirilowii. ）. In the experiment,RPLC was used in the first dimension to analyze the samples. And 12 fractions （F1 - Fl2） were obtained according to the chromatographic peak collection mode,the fractions were re-analyzed in both RPLC and SFC modes. The results clearly showed that this 2D method had good orthogonality. The SFC was used as the second dimension. Ethanol- n-hexane （3 ：7, v/v ） was used as a modifier in SFC.The modifier could provide appropriate elution power. When the sample load increased,it could also ensure the solubility of samples. The 2D RPLC/SFC method had obvious advantages for separating the compounds with similar properties,enriching and purifying the trace compo-nents. Finally,150 peaks could be detected. The off-line 2D RPLC/SFC method will be further enlarged to a preparative level for preparation of compounds. The method can provide a practi-cal reference for the purification of chemical constituents and material basis research of the seeds of T. kirilowii. in the future.

关 键 词：二维色谱 反相液相色谱 超临界流体色谱 分离 瓜蒌子 

分 类 号：O658[理学—分析化学]