College of Pharmaceutical Sciences, Zhejiang Chinese Medical University, 260 Baichuan Street, Hangzhou 311402, China.
College of Pharmaceutical Sciences, Zhejiang Chinese Medical University, 260 Baichuan Street, Hangzhou 311402, China.
J Chromatogr A. 2022 Jan 25;1663:462762. doi: 10.1016/j.chroma.2021.462762. Epub 2021 Dec 20.
Novel poly(ethylvinylbenzene-divinylbenzene) (EVB-DVB) agglomerated with ultrasmall carbonaceous spheres (UCSs) anion-exchange packings for ion chromatography (IC) were constructed. Hydrophilic UCSs with mean sizes of 62-98 nm were synthesized in quantity by the polydiallyl dimethyl ammonium chloride aided hydrothermal carbonization of fructose. The green strategy based on the thiol-ene click reaction with cysteamine in aqueous system was first designed for the hyperbranched polyquaternary amine (HPA) grafting of UCSs with negligible damage on their monodispersity. The HPA modified UCSs were evenly distributed on sulfonated EVB-DVB substrate to form one uniform layer of functional nanospheres without observable coagulum. Seven typical anions (F, Cl, NO, Br, NO, SO and PO) were baseline separated on constructed packing in 5 min with high efficiencies in the range of 44,800-71,100 plates m . The rapid separation of polarizable anions, small organic acids and saccharides could be also accomplished under isocratic elution with competitive peak symmetry and efficiency. Good reproducibility was demonstrated by consecutive injection. Thiosulfate in water reducer was further detected on prepared packing in 4 min with detection limit of 0.04 mg L (S/N = 3) and good repeatability.
新型聚(乙烯基苯-二乙烯基苯)(EVB-DVB)与超小碳质球体(UCS)阴离子交换填料的构建用于离子色谱(IC)。通过多烯丙基二甲基氯化铵辅助的果糖水热碳化合成了平均尺寸为 62-98nm 的亲水性 UCS。首次设计了基于巯基-烯点击反应与半胱胺的绿色策略,用于在水溶液中对 UCS 进行超支化聚季铵盐(HPA)接枝,对其单分散性的影响可忽略不计。改性后的 UCS 均匀分布在磺化的 EVB-DVB 基质上,形成一层均匀的功能纳米球,没有可见的凝聚物。七种典型阴离子(F、Cl、NO、Br、NO、SO 和 PO)在构建的填料上可在 5min 内基线分离,效率在 44800-71100 块/米之间。在等度洗脱条件下,也可实现对可极化阴离子、小有机酸和糖的快速分离,具有竞争峰对称性和效率。连续进样显示出良好的重现性。在制备的包装中,进一步在 4min 内检测到减水剂中的硫代硫酸盐,检测限为 0.04mg/L(S/N=3),重复性良好。