Development of new urea-functionalized silica stationary phases: Characterization and chromatographic performance

New urea-functionalized silica stationary phases were prepared by a single-step surface modification through reaction of LiChrosorb Si100 (5 μm particle size) with a homologous series of alkoxysilanes, synthesized in our laboratory, with the general formula (CH 3CH 2O) 3Si(CH 2) 3NHC(O)NH(CH 2) n CH 3, where n=4, 6 and 11. The modified silicas were characterized by elemental analysis of carbon and nitrogen, solid-state 29Si- and 13C-cross polarization magic angle spinning nuclear magnetic resonance and nitrogen adsorption isotherms at 77 K. Chromatographic evaluation of the three urea-functionalized silicas in 150×3.9 mm I.D. HPLC columns was carried out by the separation of a test mixture composed of uracil, acetophenone, benzene, toluene and naphthalene, using acetonitrile–water as mobile phase. These new stationary phases, with embedded polar urea groups, are very promising when compared with amide phases prepared by the conventional two-step modification process. A single-step reaction process silica modification is better for obtaining a well-characterized and homogeneous modified surface.