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通过原子转移自由基聚合制备的单分散热敏色谱固定相及其色谱性能

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

作者信息

Ouyang Kanglong, Cao Ying, Wang Fuqiang, Gong Bolin

机构信息

Key Laboratory of Energy & Chemical Engineering, Ningxria University, Yinchuan 750021, China.

出版信息

Se Pu. 2010 Jun;28(6):551-5. doi: 10.3724/sp.j.1123.2010.00551.

Abstract

The new monodisperse thermo-sensitive stationary phase was prepared by atom transfer radical polymerization method at room temperature using alpha-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) (P(GMA/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.

摘要

以α-溴异丁酰溴为引发剂,在室温下采用原子转移自由基聚合法,以CuCl/CuCl2/Bpy体系中形成的有机金属化合物为催化剂,制备了新型单分散热敏固定相。通过元素分析和傅里叶变换红外(FTIR)光谱对固定相进行了表征,并对其可分离性、热敏性、稳定性和重现性进行了详细评估。N-异丙基丙烯酰胺单体在聚(甲基丙烯酸缩水甘油酯-共-乙二醇二甲基丙烯酸酯)(P(GMA/EDMA))微球表面的接枝率为10.4%,该固定相通过改变温度可有效分离4-羟基苯甲醛、邻甲酚和4-正丁基苯胺。结果表明,合成的固定相具有良好的色谱性能、热敏性能和重现性。

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