title: Novel 3-hydroxypropyl-bonded phase by direct hydrosilylation of allyl alcohol on amorphous hydride silica.
abstract: A novel 3-hydroxypropyl (propanol)-bonded silica phase has been prepared by hydrosilylation of allyl alcohol on a hydride silica intermediate, in the presence of platinum (0)-divinyltetramethyldisiloxane (Karstedt's catalyst). The regio-selectivity of this synthetic approach had been correctly predicted by previous reports involving octakis(dimethylsiloxy)octasilsesquioxane (Q8 M8 (H) ) and hydrogen silsesquioxane (T8 H8 ), as molecular analogs of hydride amorphous silica. Thus, C-silylation predominated (∼94%) over O-silylation, and high surface coverages of propanol groups (5 ± 1 μmol/m(2) ) were typically obtained in this work. The propanol-bonded phase was characterized by spectroscopic (infrared (IR) and solid-state NMR on silica microparticles), contact angle (on fused-silica wafers) and CE (on fused-silica tubes) techniques. CE studies of the migration behavior of pyridine, caffeine, Tris(2,2'-bipyridine)Ru(II) chloride and lysozyme on propanol-modified capillaries were carried out. The adsorption properties of these select silanol-sensitive solutes were compared to those on the unmodified and hydride-modified tubes. It was found that hydrolysis of the SiH species underlying the immobilized propanol moieties leads mainly to strong ion-exchange-based interactions with the basic solutes at pH 4, particularly with lysozyme. Interestingly, and in agreement with water contact angle and electroosmotic mobility figures, the silanol-probe interactions on the buffer-exposed (hydrolyzed) hydride surface are quite different from those of the original unmodified tube.
authors.affiliation: Department of Chemistry, Universidad del Valle, Cali, Colombia.
authors.forename: Jorge E
authors.initials: JE
authors.lastname: Gómez
authors.forename: Fabián H
authors.initials: FH
authors.lastname: Navarro
authors.forename: Junior E
authors.initials: JE
authors.lastname: Sandoval
mesh_terms: D000433:1-Propanol; D019075:Electrophoresis, Capillary / Q000295:instrumentation* / Q000379:methods; D057927:Hydrophobic and Hydrophilic Interactions; D008956:Models, Chemical; D004364:Pharmaceutical Preparations / Q000737:chemistry / Q000302:isolation & purification; D020005:Propanols / Q000737:chemistry*; D017640:Silicates / Q000737:chemistry*
chemical_list: D004364:Pharmaceutical Preparations; D020005:Propanols; D017640:Silicates; C487012:silica hydride; C006463:allyl alcohol; D000433:1-Propanol
keywords: Bonded phases; Capillary electrophoresis; Hydrosilylation; Silica hydride; Silsesquioxanes