原子转移自由基聚合技术用于以单分散树脂为基质的温敏色谱固定相的制备及性能评价  

Monodisperse thermo-sensitive chromatographic stationary phase prepared by atom transfer radical polymerization and its chromatographic properties

作　　者：欧阳康龙[1] 曹颖[1] 王富强[1] 龚波林[1] 

机构地区：[1]宁夏大学能源化工重点实验室,宁夏银川750021

出　　处：《色谱》2010年第6期551-555,共5页Chinese Journal of Chromatography

基　　金：科技部重大基础研究前期专项基金(No.2009CB626608);国家级大学生创新实验项目资助

摘　　要：以α-溴异丁酰溴为引发剂,CuCl/CuCl2/2,2′-联二吡啶(Bpy)为催化体系,在室温条件下通过原子转移自由基聚合(ATRP)使N-异丙基丙烯酰胺(NIPAM)键合在单分散交联聚甲基丙烯酸环氧丙酯树脂(PGMA/EDMA树脂)表面,制备了具有温敏性的聚合物色谱填料,并用元素分析、红外光谱等对其进行了表征;详细考察了该填料对芳香烃化合物的分离性能、温敏性能、稳定性和重现性。元素分析得出NIPAM单体的接枝率为10.4%;通过改变温度,可以有效地分离对羟基苯甲醛、邻甲酚和4-丁基苯胺3种混合物。结果表明,所合成的固定相具有很好的色谱性能和温敏性能,稳定性和重现性良好。The new monodisperse thermo-sensitive stationary phase was prepared by atom transfer radical polymerization method at room temperature using α-bromo-isobutyryl bromide as an initiator,and the organic metal compound formed in the CuCl/CuCl2/Bpy system as a catalyst.The stationary phase was characterized by means of elementary analysis and Fourier transform infrared（FTIR） spectroscopy and evaluated in detail to determine its separability,thermosensitivity,stability and reproducibility.The grafting yield of the N-isopropylacrylamide monomer on the surface of poly（glycidyl methacrylate-co-ethylene dimethacrylate）（PGMA/EDMA） beads is 10.4%,and the stationary phase can effectively separate 4-hydroxy benzaldehyde,o-cresol and 4-n-butylaniline by changing temperature.The results showed that the synthesized stationary phase has satisfactory chromatographic properties,thermo-sensitive properties and reproducibility.

关 键 词：原子转移自由基聚合法 N-异丙基丙烯酰胺 温敏固定相 色谱性能 制备 

分 类 号：O658[理学—分析化学]