Role of the functional group in n-octydimethylsilanes in the synthesis of C8 reversed-phase silica packings for high-performance liquid chromatography

Abstract C8 reversed-phase packings have been sysnthesised by reaction of a 25-nm pore-size high-performance liquid chromatographic silica (10 μm, as(BET) = 297 m2 g-1) with 2,4-lutidine as base and dichloromethane and N,N-dimethylflormamide as solvents, or without solvents and with the following silanes: n-octyldimenthylchlorosilane (C8-Cl), n-octyldimethylhydroxysilane (C8-OH), n-octyldimethylmethoxysilane (C8-OCH3), n-octyldimethylethoxysilane (C8-OC2H5), n-octyldimethyl(dimethylamino) silane [C8-N(CH3)2], n-octyldimethyl(trifluoroacetoxy)silane (C8- OCOCF3), and bis-(n-octyldimethylsiloxane) (C8-O-C8). C8-Cl, C8-OH and C8-OCH3 each form a reactive intermediate with 2,4-lutidine, favouri…

ChemInform Abstract: Nonporous Silica Microspheres in the Micron and Submicron Size Range: Manufacture, Characterization and Application

Non-porous microparticulate supports in high-performance liquid chromatography (HPLC) of biopolymers — concepts, realization and prospects

Role of solvent and base in the silanization reaction of silicas for reversed-phase high-performance liquid chromatography

Reversed-phase packings were synthesized by reaction of n-alkyldimethylchloro- and trifluoroacetoxysilanes with silicas of 15 and 25 nm pore size, employing tetrahydrofuran, N,N-dimethylformamide, benzene, diethyl ether, dichloromethane and acetonitrile as solvents and triethylamine, pyridine, triazole, quinuclidine, 2,4- and 2,6-lutidine and imidazole as bases. With dichloromethane as solvent and 2,6- lutidine as base, n-alkyldimethyltrifluoroacetoxysilanes did not yield n-alkyl ligand densities higher than those obtained with n-alkyldimethylchlorosilanes under identical conditions. With a given base and given n-alkyldimethylchlorosilane the solvent type was found to exert a noticeable inf…

Evaluation of advanced silica packings for the separation of biopolymers by high-performance liquid chromatography

Abstract In the separation of proteins and peptides by the various modes of high-performance liquid chromatography, the nature of the substrates requires the use of microparticulate silica packings with bonded ligands of appropriate design. Agglomeration of monodisperse silica hydrosols of defined size distribution into beaded particles provides a useful method of controlling the pore size, the size distribution, the particle porosity and surface area of these packings. The particle porosity is shown to be a major factor governing the packing density and packing stability of the column. For size-exclusion chromatography of proteins, parent silicas of pore size 10 and 100 nm with a narrow po…

Separation of plasma membrane proteins of cultured human fibroblasts by affinity chromatography on bonded microparticulate silicas.

Abstract Adsorbents for high-performance affinity chromatography were prepared by bonding proteins and reactive Procion triazine dyes to 3-isothiocyanatopropyl- and 3-aminopropylsilicas. The materials prepared were used successfully in the separation of hydrophobic plasma membrane proteins of cultured human fibroblasts. The data obtained show that the reaction of 3-isothiocyanatopropyltriethoxysilane (ITCPS) with the surface hydroxyl groups of silica yields a new and convenient route to preparing an “activated carrier” that is capable of coupling with potential affinity ligands containing amino functional groups. The reaction and bonding procedures of 3-isothiocyanatopropyltriethoxysilane a…