宁夏大学能源化工重点实验室
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牛玉玲, 杨静, 董佳斌, 等. ATRP技术制备Sil-LMA反相作用色谱固定相及其性能研究[J]. 分析测试学报, 2014,33(3):283-288.
Preparation of Sil-LMA Reversed Phase Chromatographic Stationary Phase byAtom Transfer Radical Polymerization and Its Chromatographic Properties[J]. 2014,33(3):283-288.
以5 μm大孔硅胶为基质,CuBr/Bpy为催化体系,采用原子转移自由基聚合(Atom transfer radical polymerization,ATRP)技术将甲基丙烯酸月桂酯(LMA)键合到硅胶表面,制得Sil-LMA反相作用色谱固定相。采用元素分析对该固定相进行表征,以芳香族化合物为溶质,甲醇-水为流动相,对该键合相的疏水选择性进行了考察。详细研究了甲醇浓度和温度对溶质保留行为的影响,以胺类、酚类化合物为溶质,评价了其色谱性能,并计算了溶质保留过程的热力学参数。经元素分析测得该填料的接枝量高达2.323 3 mg/m2。实验结果表明,在反相模式下该固定相可基线分离5种胺类化合物和5种酚类化合物。与C18反相柱相比,该合成柱的分离时间缩短且分离效果较好。该固定相具有很好的反相色谱性能,符合反相保留机理。
Lauryl methacrylate(LMA) was grafted on the surface of 5 μm silica by atom transfer radical polymerization(ATRP) using 2-bromoisobutyryl bromide as initiator and CuBr/2,2′-bipyridyl(Bpy) as catalytic system,and a novel Sil-LMA chromatographic stationary phase was obtained.The stationary phase was characterized by elementary analysis.Hydrophobic selectivity of the Sil-LMA was evaluated by using aromatic compounds as analytes and methanol-water as binary mobile phase.Effects of methanol content in the mobile phase and temperature on chromatographic property of the stationary phase were investigated.The chromatographic property of the stationary phase was evaluated using hydroxybenzene compounds and amine compounds as solutes,and parameters of kinetics and the thermodynamics were also determined.The amount of monomer was calculated to be 2.323 3 mg/m2 on the surface of silica.The results demonstrated that the stationary phase can effectively separate five hydroxybenzene compounds and five amine compounds in RPLC mode.Compared with that of C18 column under the same chromatographic conditions,the separation efficiency of the stationary phase was better,and the analysis time was shortened.The stationary phase possessed a good reversed-phase chromatographic behavior,which was found to be well consistent with reversed-phase retention mechanism.
原子转移自由基聚合反相作用色谱胺类和酚类色谱性能
atom transfer radical polymerizationreversed phase liquid chromatography(RPLC)hydroxybenzene and amine compoundschromatographic property
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