一种表面共聚氢氧根选择性阴离子色谱固定相

A polymer resin surface polymerization-based hydroxide-selective anion exchange stationary phase

报道了一种基于聚(苯乙烯-二乙烯基苯)微球(PS-DVB)的表面共聚氢氧根选择性阴离子固定相。它以烯丙基缩水甘油醚(AGE)为功能单体、通过自由基引发直接与PS-DVB微球表面残留的悬挂双键共聚,再通过醇胺开环得到。考察了两种醇胺试剂对分离的影响;扫描电镜、红外光谱、元素分析表征结果表明:表面共聚反应成功在微球表面引入季胺基团,且对微球理化性质无显著影响;所得固定相表现氢氧根淋洗液的高选择性,对常规无机阴离子表现出良好的分离性能(分离度>1.5)和运行稳定性(保留时间的相对标准偏差<1.13%),其实用性通过分析茶叶样品中无机阴离子进行了展示。

A polystyrene-divinylbenzene(PS-DVB) microspheres-based hydroxide-selective anion exchange stationary phase is described. This stationary phase is obtained by the surface polymerization of an allyl glycidyl ether(AGE) and the pendant vinyl groups onto the surface of PS-DVB, followed by open-ring of the epoxy groups using an alkylol amine(abbreviated as P@A-M). Both alkylol amines were compared in terms of separation performance of the stationary phase. Scanning electron microscopy, infrared spectroscopy, and elemental analyses were carried out to characterize the stationary phase. The results indicated that the quaternary amine group was successfully introduced onto the surface of the PS-DVB microspheres, and that there was no obvious change in the physicochemical properties of the resin during the surface polymerization reaction. The P@A-M phase showed high hydroxide-selectivity and good separation performance(resolution>1.5) as well as high running stability(relative standard deviation of retention times<1.13%). The utility of the P@A-M phase was demonstrated by using it for the determination of inorganic anions in the tea.