title: Preparation and characterization of a poly(methyloctadecylsiloxane) thermally immobilized onto zirconized silica stationary phase for high-performance liquid chromatography.
abstract: This study describes the preparation and characterization of a HPLC stationary phase (SP) obtained by deposition of poly(methyloctadecylsiloxane) (PMODS) onto the surface of porous zirconized silica particles, followed by thermal immobilization. The SP were characterized using elemental analysis and infrared and (29)Si NMR spectroscopies, while their chromatographic behaviors were investigated by separation of selected neutral, acidic and basic compounds of different test mixtures (Engelhardt, SRM 870 and Tanaka tests). The preparation of the metalized support and the thermal immobilization of PMODS onto zirconized silica, optimized by experimental design, produced a SP based on PMODS that showed high values of efficiency (up to 85000 plates/m) and appropriate asymmetry factors. The presence of zirconium on the surface significantly decreases silica solubility in severe conditions (alkaline mobile phase at pH 10 and high temperature), increasing column lifetime.
authors.affiliation: Institute of Chemistry, University of Campinas, PO Box 6154, 13083-970 Campinas, SP, Brazil.
authors.forename: Carla G A
authors.initials: CG
authors.lastname: da Silva
authors.forename: Carol H
authors.initials: CH
authors.lastname: Collins
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006358:Hot Temperature; D006863:Hydrogen-Ion Concentration; D016062:Porosity; D012822:Silicon Dioxide / Q000737:chemistry*; D012833:Siloxanes / Q000737:chemistry*; D013499:Surface Properties; D014970:Xanthines / Q000737:chemistry; D015040:Zirconium / Q000737:chemistry*
chemical_list: C475631:Poly(methyloctadecylsiloxane); D012833:Siloxanes; D014970:Xanthines; D012822:Silicon Dioxide; D015040:Zirconium