Czech Academy of Sciences, Institute of Analytical Chemistry, Veveri 97, Brno, 60200, Czech Republic.
Czech Academy of Sciences, Institute of Analytical Chemistry, Veveri 97, Brno, 60200, Czech Republic.
J Chromatogr A. 2018 Jun 1;1552:53-59. doi: 10.1016/j.chroma.2018.04.012. Epub 2018 Apr 5.
A methodology for preparing phosphonium-based ionic liquid modified silica-based monolithic capillary columns is presented. The silica monolithic columns with dimensions of 150 × 0.1 mm were modified by a phosphonium-based ionic liquid (trioctyl(3/4-vinylbenzyl)phosphonium chloride) via 3-(trimethoxysilyl)propyl methacrylate. The prepared columns were evaluated under hydrophilic interaction liquid chromatography separation conditions, employing a sample mixture containing purine and pyrimidine bases and nucleosides. Detection was made by UV. The high efficiency of the original silica monolith was preserved even after modification, and it reached values in the range of 98,000-174,000 theoretical plates/m. The effects of the concentration of acetonitrile in the mobile phase, the presence of additives in the mobile phase, such as, acetic acid or ammonium acetate, and the pH of the mobile phase on the separation of some selected analytes were investigated. The prepared columns showed different separation selectivity compared to silica, phenyl and sulfobetaine stationary phases.
本文提出了一种制备膦基离子液体改性硅胶整体毛细管柱的方法。通过 3-(三甲氧基硅基)丙基甲基丙烯酸酯，将尺寸为 150×0.1mm 的硅胶整体柱用膦基离子液体（三辛基（3/4-乙烯基苄基）氯化膦）进行改性。在亲水相互作用液相色谱分离条件下，采用含有嘌呤和嘧啶碱基及核苷的样品混合物对制备的柱进行评价。检测采用 UV。即使在改性后，原始硅胶整体柱的高效率得以保留，其理论塔板数达到 98000-174000 范围。考察了流动相中乙腈浓度、流动相中添加剂（如乙酸或乙酸铵）的存在以及流动相 pH 值对一些选定分析物分离的影响。与硅胶、苯基和磺丁基固定相相比，制备的柱显示出不同的分离选择性。
