羧基甜菜碱型亲水作用色谱柱的制备及性能研究

发布时间：2018-07-03 12:21

本文选题：亲水作用色谱 + 固定相　；参考：《分析化学》2017年05期

【摘要】：以甲基丙烯酰氧乙基二甲基乙酸铵(CBMA)为功能单体,利用表面引发原子转移自由基聚合(Surface-initiated atom transfer radical polymerization,SI-ATRP)技术,将CBMA接枝到硅胶表面,得到接枝聚合物CBMA的亲水作用色谱固定相(Silica-CBMA)。通过改变SI-ATRP反应体系中单体的浓度,制备了3种不同接枝量的亲水作用色谱固定相。考察了Silica-CBMA固定相对有机酸类化合物的分离性能以及流动相中pH值、盐浓度、水含量等因素对溶质保留行为的影响。结果表明,在亲水作用色谱模式下,Silica-CBMA固定相对有机酸类化合物的分离是离子交换作用与亲水作用的混合色谱模式。流动相中盐浓度增大,溶质保留减弱,符合离子交换作用特征;固定相和溶质的离子化程度受流动相pH值影响较大,pH值增大,溶质保留增强;而溶质的保留时间随流动相水含量增加而降低则是典型的亲水作用色谱特征。使用自制Silica-CBMA柱,建立了芦丁片中维生素C、芦丁含量的亲水作用色谱测定方法,操作方法简单,为强极性样品的分离测定提供了新方法。
[Abstract]:Using methacryloxy ethyl dimethylammonium acetate (CBMA) as the functional monomer, the surface initiated atom transfer radical polymerization (SI-ATRP) technique was used to graft CBMA onto the silica gel surface to obtain the hydrophilic chromatographic stationary phase (Silica-CBMA) of the grafted polymer CBMA. By changing the concentration of monomer in SI-ATRP reaction system, three kinds of hydrophilic interaction chromatographic stationary phases with different grafting amount were prepared. The separation performance of Silica-CBMA fixed relative organic acids and the effects of pH value, salt concentration and water content in the mobile phase on the retention behavior of solute were investigated. The results showed that the separation of organic acids fixed by Silica-CBMA was a mixed chromatographic model of ion exchange and hydrophilicity under hydrophilic interaction chromatography mode. The concentration of salt in the mobile phase increased, the retention of solute weakened, and the ionization degree of the stationary phase and the solute was greatly affected by the pH value of the mobile phase, and the retention of solute increased. The retention time of solute decreases with the increase of water content in the mobile phase, which is a typical hydrophilic chromatographic feature. A hydrophilic chromatographic method for the determination of vitamin C and rutin in rutin tablets was established by using a self-made Silica-CBMA column. The method is simple and provides a new method for the separation and determination of highly polar samples.
【作者单位】：宁夏大学化学化工学院;北方民族大学化学与化学工程学院;
【基金】：国家自然科学基金项目(No.31360077) 宁夏自然科学基金项目(No.NZ13045)资助~~
【分类号】：O657.7

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