基于γ-环糊精和聚N-异丙基丙烯酰胺色谱固定相的制备及应用  

Preparation of Chromatographic Stationary Phase Based on γ-Cyclodextrin and Poly(N-isopropylacrylamide) and Its Application

作　　者：李媛媛[1,2] 韦嫚嫚 陈桐[3] 马玉龙[1] 

机构地区：[1]宁夏大学能源化工重点实验室,银川750021 [2]宁夏大学化学化工学院,银川750021 [3]镇江出入境检验检疫局国家食品添加剂及调味品检测重点实验室,镇江212000

出　　处：《分析化学》2015年第6期876-880,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.21465019);宁夏高等学校科学技术研究项目(No.NGY2014011);镇江市科技支撑计划项目-社会发展(No.SH2014021)项目资助~~

摘　　要：以多孔硅胶为载体,通过聚合反应将N-异丙基丙烯酰胺和甲基丙烯酸缩水甘油醚接枝于硅胶表面,并在聚合物链中植入γ-环糊精。用1H核磁共振、元素分析、红外光谱对其结构进行表征,并将此材料用作液相色谱固定相,通过考察在高亲水有机流动相中极性亲水化合物的保留,发现此固定相具有亲水色谱(HILIC)的特征,可以用于核苷类亲水化合物的分离。此外,还可以用于富勒烯碳60(C60)和碳70(C70)的分离,相比于C60,此固定相对C70有更强的保留,表明此固定相表面γ-环糊精对C70具有立体选择性。并且,此固定相具有一定的温敏特性,仅通过改变柱温就可以达到分离的目的。N-Isopropylacrylamide and glycidyl methacrylate were successfully immobilized onto the surface of porous silica particles by polymerization. Then, T-cyclodextrin was embedded in the polymer chains. The resulting material was characterized by 1H nuclear magnetic resonance, elemental analysis and FT-IR spectra and the results indicated that the new phase had been prepared successfully. The new material could be used as liquid chromatography stationary phase. By investigating the effect of the water content on the retention time of polar and hydrophilic compounds in highly organic eluents, it was found that the new material was with characteristics typical of hydrophilic interaction liquid chromatography （HILIC） and could be used to separate nucleosides compounds. Additionally, the separation of fullerenes carbon 60 （C60） and carbon 70 （C70） was achieved by using the new column. The results showed that C70 was much more strongly retained than C60 on this stationary phase, indicating that C70 had a stronger stereoselectivity interaction with T-cyclodextrin moieties than C60. Additionally, the new phase showed temperature-responsive characteristic and separation was performed by the change of column temperature.

关 键 词：亲水作用色谱 Γ-环糊精 聚N-异丙基丙烯酰胺 极性化合物 富勒烯 

分 类 号：O657.7[理学—分析化学]