Ministry of Education Key Laboratory of Analysis and Detection for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou, Fujian 350108, China.
J Chromatogr A. 2013 Jan 4;1271(1):115-23. doi: 10.1016/j.chroma.2012.11.038. Epub 2012 Nov 21.
A phenylboronic acid-silica hybrid monolithic column for capillary liquid chromatography (cLC) was prepared through one-pot process by using 4-vinylphenylboronic acid (VPBA) and alkoxysilanes simultaneously. The effects of the molar ratio of tetramethyloxysilane/γ-methacryloxypropyltrimethoxysilane (TMOS/γ-MAPS), amount of VPBA, and the volume of diethylene glycol (DEG) on the morphologies, permeabilities and pore properties of the prepared VPBA-silica hybrid monolithic columns were studied in detail. A relatively uniform monolithic structure with high porosity was obtained with optimized ingredients. A series of cis-diol-containing compounds, alkylbenzenes, amides, and anilines were utilized to evaluate the retention behaviors of the VPBA-silica hybrid monolithic column. The result demonstrated that the prepared VPBA-silica hybrid monolithic column exhibited multiple interactions including hydrophobicity, hydrophilicity, as well as cation exchange apart from the expected affinity interaction. The run-to-run, column-to-column and batch-to-batch reproducibility of the VPBA-silica hybrid monolith were satisfactory with the relative standard deviations (RSDs) less than 1.63% (n=5), 2.02% (n=3) and 2.90% (n=5), respectively, indicating the effectiveness and practicability of the proposed method. In addition, the VPBA-silica hybrid monolithic column was further applied to the separation of proteins and tryptic digest of bovine serum albumin (BSA), respectively. The successful applications suggested the potential of the VPBA-silica hybrid monolith in proteome analysis.
通过一锅法同时使用 4-乙烯基苯硼酸（VPBA）和烷氧基硅烷制备了用于毛细管液相色谱（cLC）的苯硼酸-二氧化硅杂化整体柱。详细研究了四甲氧基硅烷/γ-甲基丙烯酰氧基丙基三甲氧基硅烷（TMOS/γ-MAPS）的摩尔比、VPBA 的用量和二甘醇（DEG）的体积对制备的 VPBA-硅杂化整体柱形态、渗透性和孔性能的影响。用优化的成分获得了具有较高孔隙率的相对均匀的整体结构。利用一系列含有顺二醇的化合物、烷基苯、酰胺和苯胺来评估 VPBA-硅杂化整体柱的保留行为。结果表明，所制备的 VPBA-硅杂化整体柱除了预期的亲和相互作用外，还表现出多种相互作用，包括疏水性、亲水性和阳离子交换。VPBA-硅杂化整体柱的运行到运行、柱到柱和批到批的重现性令人满意，相对标准偏差（RSD）分别小于 1.63%（n=5）、2.02%（n=3）和 2.90%（n=5），表明该方法有效且实用。此外，VPBA-硅杂化整体柱还分别应用于蛋白质和牛血清白蛋白（BSA）胰蛋白酶消化物的分离。成功的应用表明了 VPBA-硅杂化整体柱在蛋白质组分析中的潜力。
