Preparation and evaluation of poly(4-vinylphenylboronic acid-co-pentaerythritol triacrylate) monolithic column for capillary liquid chromatography of small molecules and proteins.
Preparation and evaluation of poly(4-vinylphenylboronic acid-co-pentaerythritol triacrylate) monolithic column for capillary liquid chromatography of small molecules and proteins.
复制标题
DOI：
10.1016/j.chroma.2012.06.032
复制
发表时间：
2012-08
期刊：
影响因子：
--
通讯作者：
Huiming Huang;Zian Lin;Yao Lin;Xiaobo Sun;Yanyan Xie;Lan Zhang;Guonan Chen
中科院分区：
文献类型：
--
作者：
Huiming Huang;Zian Lin;Yao Lin;Xiaobo Sun;Yanyan Xie;Lan Zhang;Guonan Chen
研究了4-乙烯基苯基硼酸(VPBA)与季戊四醇三丙烯酸酯(PETA)在乙二醇/环己醇组成的二元致孔溶剂中的原位共聚反应，制备了一种用于毛细管色谱(CLC)的混合模式整体固定相。VPBA单体起到离子交换中心、亲水配体、疏水基团和亲和中心的作用，而PETA则被引入作为亲水交联剂。通过调整VPBA/PETA的比例和致孔溶剂的组成，优化了具有不同柱性能(如形态、渗透性和选择性)的整体柱。结果表明，单体选择性随聚合混合物中VPBA含量的增加而增加。一系列烷基苯、酰胺和苯胺被用来评价柱的疏水性、亲水性和阳离子交换作用。当最佳流速为50μL/m in(相当于0.265 mm/S)时，该整体柱对烷基苯的柱效高达43,000-100,000板/m。重现性好，批间(n=5)和柱间(n=5)保留因子的相对标准偏差(RSD)分别小于0.65%和2.49%。此外，还将聚(VPBA-co-PETA)整体柱应用于酚、碱基和蛋白质的分离。这些成功的应用表明，所设计的整体柱有望用于小分子和蛋白质的CLC分离。
A mixed-mode monolithic stationary phase was prepared for capillary liquid chromatography (cLC) by in situ copolymerization of 4-vinylphenylboronic acid (VPBA) and pentaerythritol triacrylate (PETA) in a binary porogenic solvent consisting of ethylene glycol/cyclohexanol. The monomer of VPBA functioned as ion-exchange sites, hydrophilic ligands, hydrophobic groups and affinity sites, while PETA was introduced as a hydrophilic crosslinker. The resultant monoliths with different column properties (e.g. morphology, permeability and selectivity) were optimized by adjusting the ratio of VPBA to PETA and the composition of porogenic solvent. The results showed that the selectivity of the monoliths increased with increasing content of VPBA in the polymerization mixture. A series of alkylbenzenes, amides, and anilines were used to evaluate the column performance in terms of hydrophobic, hydrophilic and cation-exchange interactions. At an optimized flow rate of 50μL/min (corresponding to 0.265mm/s), the monolith exhibited high column efficiencies of 43,000–100,000plates/m for alkylbenzenes. Good repeatability was obtained with relative standard deviation (RSD) of retention factor (k) less than 0.65% for run-to-run (n=5) and less than 2.49% for column-to-column (n=5). In addition, the poly(VPBA-co-PETA) monolithic column was applied to the separation of phenols, nucleobases, and proteins, respectively. These successful applications demonstrate the purposed monoliths are promising for cLC separation of small molecules and proteins.