氟化表面活性剂修饰硅胶色谱固定相制备及分离性能  

Fluorinated surfactant modified silica gel chromatographic stationary phase:preparation and its separation performance

作　　者：乔晓强[1] 聂扬扬 段立广[2] 梁梦颖 QIAO Xiaoqiang;NIE Yangyang;DUAN Liguang;LIANG Mengying(College of Pharmaceutical Science,Hebei University,Baoding 071002,China;Departmentof Pharmacy,The First Hospital of Hebei Medical University,Shijiazhuang 050000,China)

机构地区：[1]河北大学药学院,河北保定071002 [2]河北医科大学第一医院药学部,河北石家庄050000

出　　处：《河北大学学报（自然科学版）》2021年第5期528-534,共7页Journal of Hebei University(Natural Science Edition)

基　　金：河北省杰出青年科学基金资助项目(B2019201327);河北省百名优秀创新人才支持计划(SLRC2019016)。

摘　　要：以1-乙烯基咪唑和1-碘-1H,1H,2H,2H-全氟癸烷为原料合成了含氟表面活性剂——碘化1-乙烯基-3-全氟辛基乙基咪唑(VIMF).进一步将VIMF作为可聚合单体,利用巯基-烯点击反应,制备了VIMF键合硅胶色谱固定相(Sil-VIMF).采用傅里叶变换红外光谱和热重分析对Sil-VIMF固定相材料进行表征,结果证明了其成功制备.保留机制考察结果表明,Sil-VIMF固定相具有亲水作用色谱保留机制.色谱分离性能研究结果表明,Sil-VIMF固定相可实现酰胺类、核苷和核碱基类、苯胺类物质的良好分离,其柱效可达79200 N/m.进一步将Sil-VIMF固定相用于胃癌细胞膜脂提取物的分离分析,可实现胃癌细胞膜中磷脂酰胆碱和磷脂酰乙醇胺的有效分离分析,显示了良好的应用潜能.A fluorinated surfactant,1-vinyl-3-perfluorooctylethylimidazole iodide(VIMF),was first synthesized using 1-vinylimidazole and 1-iodo-1 H,1 H,2 H,2 H-perfluorodecane as the raw materials.With VIMF as a polymerizable monomer,VIMF bonded silica gel chromatographic stationary phase(Sil-VIMF)material was prepared by thiol-ene click reaction.Fourier transform infrared spectroscopy and thermogravimetric analysis were used for characterization the Sil-VIMF material.The results proved the successful preparation of Sil-VIMF stationary phase material.The retention mechanism investigation results show that the Sil-VIMF stationary phase has a hydrophilic interaction chromatography retention mechanism.Chromatographic separation performance results show that Sil-VIMF stationary phase can achieve good separation for amides,nucleosides/nucleobases,and anilines.The column efficiency can reach 79200 N/m.The SilVIMF stationary phase was further used for the separation and analysis of gastric cancer cell membrane lipid extracts.The effective separation and analysis of phosphatidylcholine and phosphatidylethanolamine was achieved,indicating good application potential.

关 键 词：氟表面活性剂 色谱固定相 亲水作用色谱 膜脂分离 

分 类 号：O657.7[理学—分析化学]