title: Capillary monolithic titania column for miniaturized liquid chromatography and extraction of organo-phosphorous compounds.
abstract: 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.
authors.affiliation: 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.
authors.forename: Maguy
authors.initials: M
authors.lastname: Abi Jaoudé
authors.forename: Jérôme
authors.initials: J
authors.lastname: Randon
mesh_terms: D000241:Adenosine / Q000302:isolation & purification; D002853:Chromatography, Liquid / Q000295:instrumentation*; D009943:Organophosphorus Compounds / Q000302:isolation & purification*; D044367:Phase Transition; D016062:Porosity; D012680:Sensitivity and Specificity; D012822:Silicon Dioxide / Q000737:chemistry; D013499:Surface Properties; D014025:Titanium / Q000737:chemistry*
chemical_list: D009943:Organophosphorus Compounds; C009495:titanium dioxide; D012822:Silicon Dioxide; D014025:Titanium; D000241:Adenosine