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

Research output: A Conference proceeding or a Chapter in BookConference contribution

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 (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.
Original languageEnglish
Title of host publicationACROSS Symposium on Advances in Separation Science - ASASS
Place of PublicationOnline
PublisherAustralian Centre for Research On Separation Science (ACROSS)
Pages3616-3622
Publication statusPublished - 2008
EventACROSS Symposium on Advances in Separation Science - ASASS - Hobart, Australia
Duration: 8 Dec 200810 Dec 2008

Conference

ConferenceACROSS Symposium on Advances in Separation Science - ASASS
CountryAustralia
CityHobart
Period8/12/0810/12/08

Fingerprint

Methacrylates
Liquid chromatography
Cyclodextrins
Silicon Dioxide
Cations
Polymers
Pharmaceutical Preparations
Monomers
Siloxanes
Dimethylformamide
Polycondensation
Organic solvents
Copolymerization
Optical microscopy
Methanol
Derivatives
Scanning
Scanning electron microscopy
Water

Cite this

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).
Ghanem, Ashraf. / 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. ACROSS Symposium on Advances in Separation Science - ASASS. Online : Australian Centre for Research On Separation Science (ACROSS), 2008. pp. 3616-3622
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title = "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",
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 (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.",
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booktitle = "ACROSS Symposium on Advances in Separation Science - ASASS",
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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. Australian Centre for Research On Separation Science (ACROSS), Online, pp. 3616-3622, ACROSS Symposium on Advances in Separation Science - ASASS, Hobart, Australia, 8/12/08.

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. / Ghanem, Ashraf.

ACROSS Symposium on Advances in Separation Science - ASASS. Online : Australian Centre for Research On Separation Science (ACROSS), 2008. p. 3616-3622.

Research output: A Conference proceeding or a Chapter in BookConference contribution

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AU - Ghanem, Ashraf

PY - 2008

Y1 - 2008

N2 - 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.

AB - 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.

M3 - Conference contribution

SP - 3616

EP - 3622

BT - ACROSS Symposium on Advances in Separation Science - ASASS

PB - Australian Centre for Research On Separation Science (ACROSS)

CY - Online

ER -

Ghanem A. 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. Online: Australian Centre for Research On Separation Science (ACROSS). 2008. p. 3616-3622