Liu Junwei, Wang Yong, Cheng Heli, Wang Nani, Wu Shuchao, Zhang Peimin, Zhu Yan
Department of Chemistry, Xixi Campus, Zhejiang University, Hangzhou 310028, China.
Institute of Forensic Science and Technology of Nanjing Public Security Bureau, Nanjing 210001, China.
Talanta. 2016 Oct 1;159:272-279. doi: 10.1016/j.talanta.2016.06.034. Epub 2016 Jun 18.
Poly (glycidylmethacrylate-divinylbenzene) microspheres were prepared by the two-staged swelling and polymerization method and applied to prepare anion exchange stationary phases. Methylamine, dimethylamine, trimethylamine, diethylamine and triethylamine were selected to prepare the quaternary ammonium groups of anion exchangers, respectively. The diameters and surface characteristics of microspheres were measured by scanning electron microscope and nitrogen adsorption-desorption measurements. The anion exchangers were characterized by Fourier transform infrared spectrum, elemental analysis and breakthrough curve methods. The chromatographic performances of anion exchangers were illustrated by separating conventional anions, organic weak acids and carbohydrates. The results indicated that the anion exchange capacities were controllable by changing either the content of glycidylmethacrylate in microspheres or the number of bonded quaternary ammonium layer. Meanwhile, the substituents of quaternary ammonium groups greatly influenced the separation properties of anion exchangers. Finally, the three-layer methylamine-quaternized anion exchanger was successfully applied for the determination of fluoride in tea sample. The content of fluoride was detected to be 0.13mgg(-1) without the interference of acetate and formate.
采用两步溶胀聚合方法制备了聚(甲基丙烯酸缩水甘油酯 - 二乙烯基苯)微球,并将其应用于制备阴离子交换固定相。分别选用甲胺、二甲胺、三甲胺、二乙胺和三乙胺制备阴离子交换剂的季铵基团。通过扫描电子显微镜和氮吸附 - 脱附测量来测定微球的直径和表面特性。利用傅里叶变换红外光谱、元素分析和穿透曲线方法对阴离子交换剂进行表征。通过分离常规阴离子、有机弱酸和碳水化合物来说明阴离子交换剂的色谱性能。结果表明,通过改变微球中甲基丙烯酸缩水甘油酯的含量或键合季铵层的数量,阴离子交换容量是可控的。同时,季铵基团的取代基对阴离子交换剂的分离性能有很大影响。最后,三层甲胺季铵化阴离子交换剂成功应用于茶叶样品中氟化物的测定。检测到氟化物含量为0.13mg g(-1),不受乙酸盐和甲酸盐的干扰。