title: Preparation and characterization of long alkyl chain methacrylate-based monolithic column for capillary chromatography.
abstract: This paper describes the fabrication of long alkyl chain methacrylate monolithic materials for using as stationary phases in capillary liquid chromatography. Following deactivation of the capillary surface with 3-(trimethoxysilyl)propyl methacrylate (gamma-MAPS), monoliths were formed by co-polymerisation of stearyl methacrylate (SMA) with ethylene glycol dimethacrylate (EDMA) in the presence of the initiator AIBN and a mixture of porogens including iso-amyl alcohol and 1,4-butanediol. The monoliths were prepared in 100 microm i.d. capillaries and the composition of the polymerisation mixtures were optimised in terms of the ratio of SMA/EDMA, the porogen composition and ratio of porogen to monomers. As the porogen weight fraction decreased, the microglobules became smaller and as expected, the total porosity decreased. In order to determine the usability of such materials, the column permeability K was measured by pumping water through the columns at different linear flow rates. Good results were obtained when these capillaries were used to separate mixtures of weak acids, neutral and basic compounds.
authors.affiliation: Pharmaceutical Sciences Research Division, King's College London, SE1 9NH, UK.
authors.forename: Zhengjin
authors.initials: Z
authors.lastname: Jiang
authors.forename: Norman William
authors.initials: NW
authors.lastname: Smith
authors.forename: Paul David
authors.initials: PD
authors.lastname: Ferguson
authors.forename: Mark Robert
authors.initials: MR
authors.lastname: Taylor
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D008689:Methacrylates / Q000138:chemical synthesis; D008855:Microscopy, Electron, Scanning; D010636:Phenols / Q000302:isolation & purification; D011084:Polycyclic Aromatic Hydrocarbons / Q000302:isolation & purification
chemical_list: D008689:Methacrylates; D010636:Phenols; D011084:Polycyclic Aromatic Hydrocarbons