Mixed-mode silica monolith as an efficient separation medium for capillary electrochromatography

Silica monolith column having mixed-mode i.e., hydrophobic (C18) and anion exchange interaction was successfully synthesized by on-column modification of the hybrid tetramethoxysilanes (TMOS) and methyltrimethoxysilanes (MTMS) using octadecyldimethyl-(N-N-diethylamino)silane (ODS) and ion exchange m...

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Main Author:	Jemale, Alia Sofie
Format:	Thesis
Language:	English
Published:	2010
Subjects:	T Technology (General) TP Chemical technology
Online Access:	http://eprints.utm.my/id/eprint/12364/9/AliaSofieJemaleMFSA2010.pdf
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spelling	my-utm-ep.123642017-09-17T08:17:25Z Mixed-mode silica monolith as an efficient separation medium for capillary electrochromatography 2010 Jemale, Alia Sofie T Technology (General) TP Chemical technology Silica monolith column having mixed-mode i.e., hydrophobic (C18) and anion exchange interaction was successfully synthesized by on-column modification of the hybrid tetramethoxysilanes (TMOS) and methyltrimethoxysilanes (MTMS) using octadecyldimethyl-(N-N-diethylamino)silane (ODS) and ion exchange monomer of N-[3-(dimethylamino)propyl]acrylamide (DMAPAA-Q) methyl chloride-quaternary salt, for the surface modification. The preparation of the ODS/DMAPAA-Q silica monolith column was carried out in a fused silica capillary column of 75 µm internal diameter. At each modification stage, the ODS/DMAPAA-Q silica monolith column was chromatographically characterized with micro liquid chromatography (µLC) and produced separation efficiencies of up to 43000 plates/min at the optimum velocity using the test mixture of alkylbenzenes, and 41800 plates/min for selected nucleotides. The ODS/DMAPAA-Q silica monolith column was also characterized physically with scanning electron microscope (SEM), and showed to have an average through-pore size and skeleton size of 2.2 µm and 2.0 µm, respectively. The ODS/DMAPAA-Q silica monolith column was then characterized in capillary electrochromatography (CEC) for the separation of inorganic and organic ions using a 50 mM phosphate pH 6.9 background electrolyte. The inorganic anions and organic ions were separated within 10 mins with column efficiency up to 114900 plates/min. The results suggest that modifying a silica monolith capillary column through in-situ polymerization of a monomer carrying a functional group can yield high efficiency columns for the ion-exchange-mode separation as well as for reversed-phased separations. The analysis of the porous silica monolith columns with CEC yields higher performance than CZE analysis for the separation of anions. 2010 Thesis http://eprints.utm.my/id/eprint/12364/ http://eprints.utm.my/id/eprint/12364/9/AliaSofieJemaleMFSA2010.pdf application/pdf en public masters Universiti Teknologi Malaysia, Faculty of Science Faculty of Science
institution	Universiti Teknologi Malaysia
collection	UTM Institutional Repository
language	English
topic	T Technology (General) TP Chemical technology
spellingShingle	T Technology (General) TP Chemical technology Jemale, Alia Sofie Mixed-mode silica monolith as an efficient separation medium for capillary electrochromatography
description	Silica monolith column having mixed-mode i.e., hydrophobic (C18) and anion exchange interaction was successfully synthesized by on-column modification of the hybrid tetramethoxysilanes (TMOS) and methyltrimethoxysilanes (MTMS) using octadecyldimethyl-(N-N-diethylamino)silane (ODS) and ion exchange monomer of N-[3-(dimethylamino)propyl]acrylamide (DMAPAA-Q) methyl chloride-quaternary salt, for the surface modification. The preparation of the ODS/DMAPAA-Q silica monolith column was carried out in a fused silica capillary column of 75 µm internal diameter. At each modification stage, the ODS/DMAPAA-Q silica monolith column was chromatographically characterized with micro liquid chromatography (µLC) and produced separation efficiencies of up to 43000 plates/min at the optimum velocity using the test mixture of alkylbenzenes, and 41800 plates/min for selected nucleotides. The ODS/DMAPAA-Q silica monolith column was also characterized physically with scanning electron microscope (SEM), and showed to have an average through-pore size and skeleton size of 2.2 µm and 2.0 µm, respectively. The ODS/DMAPAA-Q silica monolith column was then characterized in capillary electrochromatography (CEC) for the separation of inorganic and organic ions using a 50 mM phosphate pH 6.9 background electrolyte. The inorganic anions and organic ions were separated within 10 mins with column efficiency up to 114900 plates/min. The results suggest that modifying a silica monolith capillary column through in-situ polymerization of a monomer carrying a functional group can yield high efficiency columns for the ion-exchange-mode separation as well as for reversed-phased separations. The analysis of the porous silica monolith columns with CEC yields higher performance than CZE analysis for the separation of anions.
format	Thesis
qualification_level	Master's degree
author	Jemale, Alia Sofie
author_facet	Jemale, Alia Sofie
author_sort	Jemale, Alia Sofie
title	Mixed-mode silica monolith as an efficient separation medium for capillary electrochromatography
title_short	Mixed-mode silica monolith as an efficient separation medium for capillary electrochromatography
title_full	Mixed-mode silica monolith as an efficient separation medium for capillary electrochromatography
title_fullStr	Mixed-mode silica monolith as an efficient separation medium for capillary electrochromatography
title_full_unstemmed	Mixed-mode silica monolith as an efficient separation medium for capillary electrochromatography
title_sort	mixed-mode silica monolith as an efficient separation medium for capillary electrochromatography
granting_institution	Universiti Teknologi Malaysia, Faculty of Science
granting_department	Faculty of Science
publishDate	2010
url	http://eprints.utm.my/id/eprint/12364/9/AliaSofieJemaleMFSA2010.pdf
_version_	1747814929291804672

Mixed-mode silica monolith as an efficient separation medium for capillary electrochromatography

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