Perphenylcarbamoylated β-cyclodextrin-silica (Ph-β-CD-silica) hybrid monolithic columns for enantioseparation in capillary liquid chromatography (cLC) have been prepared by a “one-pot” approach via the polycondensation of alkoxysilanes and in situ copolymerization of mono (6A-N-allylamino-6A-deoxy)-Ph-β-CD and vinyl group on the precondensed siloxanes. The morphologies of the Ph-β-CD-silica hybrid monolithic columns were characterized by optical microscopy and scanning electron microscopy (SEM), showing the uniform monolithic matrixes tightly bonded onto the capillary wall. The content of Ph-β-CD incorporated in monolithic matrix by the “one-pot” approach was ca. 2.9 times higher than that by postmodification method. The permeability of the Ph-β-CD-silica chiral hybrid monolithic column was 3.63 × 10−14 m2, and the minimum plate height was 12 μm corresponding to 83 300 theoretical plates/meter. Enantioseparations of 13 racemates were achieved by the Ph-β-CD-silica hybrid monolithic column. In this work, since the prepolymerization system mainly consisted of organic solvent (methanol (MeOH), N,N-dimethylformamide (DMF)), the limitation and difficulty of the use of water insoluble organic monomers in the previously reported “one-pot” method was circumvented. Therefore, various β-CD derivatives as well as other hydrophobic monomers could thus be used to prepare organic−silica hybrid monolithic columns with the “one-pot” process.
|Title of host publication||ACROSS Symposium on Advances in Separation Science - ASASS|
|Place of Publication||Online|
|Publisher||Australian Centre for Research On Separation Science (ACROSS)|
|Publication status||Published - 2008|
|Event||ACROSS Symposium on Advances in Separation Science - ASASS - Hobart, Australia|
Duration: 8 Dec 2008 → 10 Dec 2008
|Conference||ACROSS Symposium on Advances in Separation Science - ASASS|
|Period||8/12/08 → 10/12/08|
Ghanem, A. (2008). Preparation of Reversed-phase And Cation-exchange Mixed-mode Porous Sulfopropyl Methacrylate Polymer-based Monolithic Capillary For The Separation Of Pharmaceutical Compounds Using Capillary-Liquid Chromatography. In ACROSS Symposium on Advances in Separation Science - ASASS (pp. 3616-3622). Online: Australian Centre for Research On Separation Science (ACROSS).