Laboratoire des Sciences Analytiques, Université Claude Bernard Lyon 1, Université de Lyon, Bâtiment Curien, LSA, 43 Boulevard du 11 Novembre 1918, 69622 Villeurbanne Cedex, France.
Anal Bioanal Chem. 2011 May;400(5):1241-9. doi: 10.1007/s00216-011-4681-4. Epub 2011 Feb 18.
A new sol-gel protocol was designed and optimized to produce titanium-dioxide-based columns within confined geometries such as monolithic capillary columns and porous-layer open-tubular columns. A surface pre-treatment of the capillary enabled an efficient anchorage of the monolith to the silica capillary wall during the synthesis. The monolith was further synthesized from a solution containing titanium n-propoxide, hydrochloric acid, N-methylformamide, water, and poly(ethylene oxide) as pore template. The chromatographic application of capillary titania-based columns was demonstrated with the separation of a set of phosphorylated nucleotides as probe molecules using aqueous normal-phase liquid chromatography conditions. Capillary titania monoliths offered a compromise between the high permeability and the important loading capacity needed to potentially achieve miniaturized sample preparations. The specificity of the miniaturized titania monolithic support is illustrated with the specific enrichment of 5'-adenosine mono-phosphate. The monolithic column offered a ten times higher loading capacity of 5'-adenosine mono-phosphate compared with that of the capillary titania porous-layer open-tubular geometry.
设计并优化了一种新的溶胶-凝胶方案，以在受限的几何形状内生产基于二氧化钛的柱体，例如整体式毛细管柱和多孔层开管柱。对毛细管进行表面预处理，可在合成过程中实现将整体式固定相有效地锚定到硅胶毛细管壁上。整体式固定相进一步由含有钛正丙氧基化物、盐酸、N-甲基甲酰胺、水和聚（氧化乙烯）作为孔模板的溶液合成。使用水相正相液相色谱条件，以一组磷酸化核苷酸作为探针分子，展示了基于毛细管二氧化钛柱的色谱应用。毛细管二氧化钛整体式柱在高渗透性和实现微型化样品制备所需的重要载样量之间提供了折衷。微型化二氧化钛整体式支撑物的特异性通过 5'-腺苷一磷酸的特异性富集得到说明。与毛细管二氧化钛多孔层开管几何形状相比，整体式柱可对 5'-腺苷一磷酸进行 10 倍的高载样量富集。
