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Preparation of polymer monolithic column functionalized by arsonic acid groups for mixed-mode capillary liquid chromatography
Journal of Chromatography A ( IF 3.8 ) Pub Date : 2018-03-05 , DOI: 10.1016/j.chroma.2018.03.007
Zhang-Na Qin , Qiong-Wei Yu , Ren-Qi Wang , Yu-Qi Feng

A mixed-mode polymer monolithic column functionalized by arsonic acid groups was prepared by single-step in situ copolymerization of monomers p-methacryloylaminophenylarsonic acid (p-MAPHA) and pentaerythritol triacrylate (PETA). The prepared poly(p-MAPHA-co-PETA) monolithic column has a homogeneous monolithic structure with good permeability and mechanical stability. Zeta potential measurements reveal that the monolithic stationary phase holds a negative surface charge when the mobile phase resides in the pH range of 3.0–8.0. The retention mechanisms of prepared monolithic column are explored by the separation of selected polycyclic aromatic hydrocarbons (PAHs), nucleosides, and three basic compounds. The results indicate that the column functions in three different separation modes associated with reversed-phase chromatography based on hydrophobic interaction, hydrophilic interaction chromatography, and cation-exchange chromatography. The column efficiency of prepared monolithic column is estimated to be 70,000 and 76,000 theoretical plates/m for thiourea and naphthalene, respectively, at a linear flow velocity of 0.85 mm/s using acetonitrile/H2O (85/15, v/v) as the mobile phase. Furthermore, an analysis of the retention factors obtained for the PAHs indicates that the prepared monolithic column exhibits good reproducibility with relative standard deviations of 2.9%, 4.0%, and 4.7% based on run-to-run injections, column-to-column preparation, and batch-to-batch preparation, respectively. Finally, we investigate the separation performance of the proposed monolithic column for select phenols, sulfonamides, nucleobases and nucleosides.



中文翻译:

砷酸基官能化的聚合物整体柱用于混合模式毛细管液相色谱的制备

通过单步原位共聚单体甲基丙烯酸丙烯酰氨基苯基ar酸(p- MAPHA)和季戊四醇三丙烯酸酯(PETA),制备了由砷酸基团官能化的混合模式聚合物整体柱。制备的聚(p -MAPHA- co-PETA)整体柱具有均匀的整体结构,具有良好的渗透性和机械稳定性。Zeta电势测量表明,当流动相的pH范围为3.0-8.0时,整体固定相具有负表面电荷。通过选择的多环芳烃(PAHs),核苷和三种碱性化合物的分离,探索了制备的整体柱的保留机理。结果表明,该色谱柱在基于疏水相互作用,亲水相互作用色谱和阳离子交换色谱的反相色谱分析中以三种不同的分离模式起作用。对于硫脲和萘,制备的整体柱的柱效估计分别为70,000和76,000理论塔板/ m,2 O(85/15,v / v)作为流动相。此外,对获得的多环芳烃的保留因子的分析表明,所制备的整体式色谱柱具有良好的重现性,基于每次进样,色谱柱到色谱柱的制备,相对标准偏差为2.9%,4.0%和4.7%。 ,以及批次之间的准备。最后,我们研究了所提出的整体式色谱柱对某些酚,磺酰胺,核苷碱基和核苷的分离性能。

更新日期:2018-03-05
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