0000000000204783
AUTHOR
Michael Hanson
A model for polybutadiene coatings on porous silica
Non-wetting viscous liquids such as oligobutadiene prefer “active” sites such as pores during the process of physisorption. Thus, polybutadiene (PBD) coatings on porous silica do not result in a homogeneous polymer film but in an inhomogeneous loading where the bulk polymer is mainly sited in the pores of the silica. An increasing polymer loading leads to increasingly filled pores instead of a thicker polymer film. We cannot exclude the possibility that most of the surface is covered at least with a thin polymer film since the chromatographic behaviour is relatively good for polypeptides, which are highly susceptible to the silanol groups of silica.
Polymer-coated reversed-phase packings with controlled hydrophobic properties
Abstract We have designed and synthesized novel reversed-phase packings of non-porous and porous polymethacrylate-coated silicas. By varying the hydrophobicity of the polymer coating, selective unfolding of polypeptides may be achieved, thus enabling manipulation of the chromatographic profile. This study characterizes these packings through their employment for separations of model synthetic peptides of defined secondary, tertiary and quaternary structure. Thus, the packings were applied to the reversed-phase separation α-helical amphipathic and non-amphipathic peptides of the same amino acid composition but different sequences. In addition, selective unfolding of model to-stranded α-helic…
Polymer-coated reversed-phase packings in high-performance liquid chromatography
The synthesis and properties of polymer-coated RP stationary phases are reviewed. The sorbents are classified according to the method of synthesis. More flexibility in the tailoring of polymer-coated packings is noted. The impact of the polymer coating on the porosity of the oxides to be modified and their chromatographic properties is discussed.
Interactions of lysozyme with hydrophilic and hydrophobic polymethacrylate stationary phases in reversed phase chromatography (RPC)
Two silicas, one with a mean pore diameter of 30 nm and the other non-porous, were coated with polymethacrylates of increasing hydrophobicity in the sequence: poly-2-hydroxyethylmethacrylate (P2HEMA)1 polyethylmethacrylate (PEMA) and poly-n-octylmethacrylate (POMA). Association constants, Kass, between lysozyme and the coated silicas were determined by means of frontal analysis, and the apparent heats of adsorption, delta Happ, by means of microcalorimetry. Using Kass and delta Happ the changes in the apparent free energy, delta Gapp, and in the apparent entropy, delta Sapp, were calculated at a concentration of lysozyme < 10 mumol/l. The association between the lysozyme and the coated sili…
Non-porous polybutadiene-coated silicas as stationary phases in reversed-phase chromatography
Abstract Non-porous silica of mean particle diameter 1.7 μm (Monospher) was coated with polybutadiene (PBD) following a published procedure. The silicas were prepared with graduated polymer loads up to 8% (w/w). Examination of the PBD-coated packings by means of electron spectroscopy for chemical analysis, scanning electron microscopy, diffuse reflection infrared fourier transform spectroscopy and differential thermal gravimetry indicated that the optimum polymer load was between 1 and 3% (w/w) with regard to a dense coverage corresponding to an average layer thickness of about 4 nm. No silanophilic interactions could be monitored using 1–3% (w/w) coated silicas under reversed-phase conditi…