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…

BONDED SILICA PHASES FOR THE SEPARATION OF BIOPOLYMERS BY MEANS OF COLUMN LIQUID CHROMATOGRAPHY

Retention behaviour of paracelsin peptides on reversed-phase silicas with varying n-alkyl chain length and ligand density.

As part of further investigations on the characterization of the ligand-induced conformational stabilization of peptides, two series of n-alkyldimethylsilyl bonded silicas have been prepared. In series A the n-alkyl chain length, n, of the bonded phase was varied between 1 and 20 carbon atoms at a constant ligand density. In series B the ligand density, alpha exp, was gradually changed from 0 to 4.1 mumol/m2 on a C1, C4, C6, C8 and C18 bonded phase. The retention behaviour of four peptides of the paracelsin family were examined under isocratic conditions, using a ternary mobile phase of water-methanol-acetonitrile (22:39:39, v/v/v). Plots of k' versus n showed pronounced maxima between n = …

Impact of acidic/hydrothermal treatment on pore structural and chromatographic properties of porous silicas

Abstract A series of commercial silicas and a laboratory made product were subjected to acidic/hydrothermal treatment with solutions of HCI, HNO3, H2SO4 and HF. The concentration of acid and the temperature and duration of treatment were varied. The specific surface area, content of metal impurities, types and concentration of surface hydroxyl and siloxane groups and crystallinity were determined for native and treated silicas. Only changes in the structural order of the surface could be assessed by means of 19Si cross-polarization magic angle spinning NMR spectrometry and electron diffraction. The native and acid-treated silicas were surface modified to n-octyl derivatives and tested under…