详细信息

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.

文献类型:期刊文献

中文题名: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

英文题名: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[1];彭子悦[1];傅青[1];金郁[1]

机构:[1]华东理工大学药学院,上海200237

年份:2017

卷号:35

期号:7

起止页码:683

中文期刊名:色谱

外文期刊名:Chinese Journal of Chromatography

收录:CSTPCD;;Scopus;WOS:【ESCI(收录号:WOS:000411256800002)】;北大核心:【北大核心2014】;CSCD:【CSCD2017_2018】;PubMed;

基金:National Natural Science Foundation of China (No. 21305138).

语种:中文

中文关键词:二维色谱;反相液相色谱;超临界流体色谱;分离;瓜蒌子

外文关键词:two dimensional (2D ) chromatography; reversed-phase liquid chromatography (RPLC); supercritical fluid chromatography (SFC); separation; the seeds of Trichosanthes kirilowii Maxim. ( T. kirilowii. )

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.

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