Preparation of phenyl-silica hybrid monolithic column with "one-pot" process for capillary liquid chromatography.
Preparation of phenyl-silica hybrid monolithic column with "one-pot" process for capillary liquid chromatography.
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DOI：
10.1016/j.chroma.2011.07.048
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发表时间：
2012-03
期刊：
影响因子：
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通讯作者：
Zhenbin Zhang;Hui Lin;Junjie Ou;Hongqiang Qin;R. Wu;Jing Dong;Hanfa Zou
中科院分区：
文献类型：
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作者：
Zhenbin Zhang;Hui Lin;Junjie Ou;Hongqiang Qin;R. Wu;Jing Dong;Hanfa Zou
以甲基丙烯酸苄酯和烷氧基硅烷为原料，采用“一锅法”制备了毛细管液相色谱用苯基-硅杂化整体柱。考察了四甲基氧基硅烷/乙烯基三甲氧基硅烷的摩尔比（TMOS/VTMS）、缩聚温度、超分子模板（十六烷基三甲基溴化铵，CTAB）含量、N、N′-二甲基甲酰胺/甲醇的比例（v/v）、甲基丙烯酸苄酯的体积对制备的苯基-二氧化硅杂化整体柱形貌的影响。计算得到混合整体柱的渗透率为3.23×10−13m2，最小板高为8.38μm，相当于每米119000块理论板。在混合整体柱上实现了多种中性、极性和碱性分析物以及小肽的分离，具有较高的效率和良好的重现性。此外，将所制备的杂交整体柱应用于牛血清白蛋白（BSA）、卵白蛋白、α-酪蛋白、细胞色C和肌红蛋白的串联质谱（cLC - MS/MS）分析，结果表明其分离性能接近十八烷基硅烷（C18）填充毛细管柱，显示了其在蛋白质组学分析中的潜力。此外，由于预聚合体系主要由有机溶剂（甲醇和N，N ' -二甲基甲酰胺）组成，因此各种疏水单体可以通过“一锅法”制备有机硅杂化整体柱。
A phenyl-silica hybrid monolithic column for capillary liquid chromatography (cLC) was prepared through “one-pot” process by con-currently using benzyl methacrylate and alkoxysilanes. The effects of the molar ratio of tetramethoxysilane/vinyltrimethoxysilane (TMOS/VTMS), polycondensation temperature, content of supramolecule template (cetyltrimethylammonium bromide, CTAB), ratio of N,N′-dimethylformamide/methanol (v/v), the volume of benzyl methacrylate on the morphologies of the prepared phenyl-silica hybrid monolithic columns were investigated in detail. The permeability of the hybrid monolithic column was calculated as 3.23×10−13m2, and the minimum plate height was determined as 8.38μm which corresponding to 119,000 theoretical plates per meter. Separation of various neutral, polar and basic analytes as well as small peptides on the hybrid monolithic column was achieved by cLC and showed high efficiency and satisfactory reproducibility. Moreover, the prepared hybrid monolithic column was also applied for the analysis of tryptic digests of bovine serum albumin (BSA), ovalbumin, α-casein, cytochrome C and myoglobin by cLC tandem mass spectrometry (cLC–MS/MS), and the results showed that the separation performance was close to that of the octadecylsilane (C18) packed capillary column which demonstrating its potential in proteome analysis. Moreover, since the prepolymerization system was mainly consisted of organic solvents (methanol and N,N′-dimethylformamide), various hydrophobic monomers could be potentially used to prepare organic-silica hybrid monolithic columns through “one-pot” approach.