Preparation and Application of Weak Cation Exchange Resin Based on Thiol Click Reaction

IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL
Zhongping Huang, Qingqing Zhu, Yu Han, Ying Mo, Junhao Zhang, Huijun Liu
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Abstract

Using poly(styrene-divinylbenzene) microspheres as stationary phase matrix and mercaptosuccinic acid as a modifier, a new weak cation exchange resin was synthesized by thiol click reaction. The conditions for thiol-chlorine click reaction and thiol-alkene click reaction were optimized. The surface morphology and chemical composition of the modified microspheres were characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, and an elemental analyzer. The stationary phase can achieve the separation of six common cations within 25 min. A homemade weak cation chromatographic column was used to determine the impurities of Na+ and K+ and the content of tetramethylammonium ions in tetramethylammonium hydroxide samples. The method showed a good linear correlation in the range of 0.1–500.0 mg/L with correlation coefficients of 0.9998–0.9999, and the limits of detection (signal-to-noise ratio ≥ 3) were 0.01–0.20 mg/L. The intra-day relative standard deviations (RSDs) were in the range of 1.1%–4.4%, and the inter-day RSDs were in the range of 0.8%–14.8%. The spiked recoveries were in the range of 91.92%–119.86%. The results showed that the prepared stationary phase exhibited effective separation ability and good reproducibility, which was suitable for the analysis of the impurities of Na+, K+, and the content of tetramethylammonium in the tetramethylammonium reagents.

基于硫醇点击反应的弱阳离子交换树脂的制备与应用。
以聚(苯乙烯-二乙烯基苯)微球为固定相基质,以巯基丁二酸为改性剂,通过硫醇点击反应合成了一种新型弱阳离子交换树脂。对硫醇-氯点击反应和硫醇-烯点击反应的条件进行了优化。通过扫描电子显微镜、傅立叶变换红外光谱和元素分析仪对改性微球的表面形貌和化学成分进行了表征。该固定相可在 25 分钟内实现六种常见阳离子的分离。利用自制的弱阳离子色谱柱测定了四甲基氢氧化铵样品中的 Na+、K+ 杂质和四甲基铵离子含量。该方法在0.1-500.0 mg/L范围内线性关系良好,相关系数为0.9998-0.9999,检出限(信噪比≥3)为0.01-0.20 mg/L。日内相对标准偏差(RSD)为 1.1%-4.4%,日间 RSD 为 0.8%-14.8%。加标回收率在 91.92%-119.86% 之间。结果表明,所制备的固定相具有有效的分离能力和良好的重现性,适用于分析四甲基铵试剂中的杂质 Na+、K+ 和四甲基铵的含量。
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来源期刊
Journal of separation science
Journal of separation science 化学-分析化学
CiteScore
6.30
自引率
16.10%
发文量
408
审稿时长
1.8 months
期刊介绍: The Journal of Separation Science (JSS) is the most comprehensive source in separation science, since it covers all areas of chromatographic and electrophoretic separation methods in theory and practice, both in the analytical and in the preparative mode, solid phase extraction, sample preparation, and related techniques. Manuscripts on methodological or instrumental developments, including detection aspects, in particular mass spectrometry, as well as on innovative applications will also be published. Manuscripts on hyphenation, automation, and miniaturization are particularly welcome. Pre- and post-separation facets of a total analysis may be covered as well as the underlying logic of the development or application of a method.
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