title: Preparation of perphenylcarbamoylated β-cyclodextrin-silica hybrid monolithic column with "one-pot" approach for enantioseparation by capillary liquid chromatography.
abstract: 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 (6(A)-N-allylamino-6(A)-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) m(2), 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.
authors: Key Laboratory of Separation Science for Analytical Chemistry, National Chromatographic R & A Center, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, China.
authors: Zhenbin
authors: Z
authors: Zhang
authors: Minghuo
authors: M
authors: Wu
authors: Ren'an
authors: R
authors: Wu
authors: Jing
authors: J
authors: Dong
authors: Junjie
authors: J
authors: Ou
authors: Hanfa
authors: H
authors: Zou
mesh_terms: D005591:Chemical Fractionation / Q000379:methods*; D002853:Chromatography, Liquid / Q000379:methods*; D056148:Chromatography, Reverse-Phase; D008958:Models, Molecular; D008968:Molecular Conformation; D058105:Polymerization; D012821:Silanes / Q000737:chemistry; D012822:Silicon Dioxide / Q000737:chemistry*; D013237:Stereoisomerism; D047392:beta-Cyclodextrins / Q000737:chemistry*
chemical_list: D012821:Silanes; D047392:beta-Cyclodextrins; D012822:Silicon Dioxide