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Hydrophilic Separation Materials for Liquid Chromatography
Umeå University, Faculty of Science and Technology, Chemistry.
2007 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The main focus of this thesis is on hydrophilic interaction chromatography (HILIC) and the preparation of stationary phases for HILIC. The mechanism of HILIC is also discussed; a large part of the discussion has been adapted from a review written by me and professor Irgum for the Journal of Separation Science (ref 34). By reevaluating the literature we have revealed that the notion of HILIC as simply partitioning chromatography needed modification. However, our interest in the HILIC mechanism was mainly inspired by the need to understand how to construct the optimal HILIC stationary phase. The ultimate stationary phase for HILIC is still not found. My theory is that a non-charged stationary phase capable of retaining a full hydration layer even at extreme acetonitrile (> 85%) concentrations should give a HILIC stationary phase with a more pure partitioning retention behavior similar to that of a swollen C18 reversed phase. The preparation of a sorbitol methacrylate grafted silica stationary phase is one of our attempts at producing such a stationary phase. The preparation of such a grafted silica has been performed, but with huge difficulty and this work is still far from producing a column of commercial quality and reprodicibility.

This thesis also discusses a new method for the initiation of atom transfer radical polymerization from chlorinated silica. This new grafting scheme theoretically results in a silica particle grafted with equally long polymer chains, anchored to the silica carrier by a hydrolytically stable silicon-carbon bond. The hydrolytic stability is especially important for HILIC stationary phases due to the high water concentration at the surface.

Place, publisher, year, edition, pages
Umeå: Kemi , 2007. , 24 p.
Keyword [en]
Chromatography, HILIC, Hydrophilic, Stationary phase
National Category
Chemical Sciences
Identifiers
URN: urn:nbn:se:umu:diva-1350ISBN: 978-91-7264-406-9 (print)OAI: oai:DiVA.org:umu-1350DiVA: diva2:140730
Public defence
2007-10-05, KB3A9, KBC-Huset, Umeå Universitet, Umeå, 10:00 (English)
Opponent
Supervisors
Available from: 2007-09-14 Created: 2007-09-14 Last updated: 2009-09-17Bibliographically approved
List of papers
1. Polymer-based monolithic microcolumns for hydrophobic interaction chromatography of proteins.
Open this publication in new window or tab >>Polymer-based monolithic microcolumns for hydrophobic interaction chromatography of proteins.
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2006 (English)In: Journal of Separation Science, ISSN 1615-9306, Vol. 29, no 1, 25-32 p.Article in journal (Refereed) Published
Abstract [en]

Monolithic capillary columns for hydrophobic interaction chromatography (HIC) have been prepared by thermally initiated, single-step in situ polymerization of mixtures of monovinyl monomers including butyl methacrylate and/or 2-hydroxyethyl methacrylate, with a divinyl crosslinker glycerol dimethacrylate or 1,4-butanediol dimethacrylate using two different porogen systems. Two porogenic solvent mixtures were used; one "hydrophilic", consisting of water, butanediol, and propanol, and one "hydrophobic," comprising dodecanol and cyclohexanol. The porous structures of the monoliths were characterized and their performance was demonstrated with a separation of a mixture of myoglobin, ribonuclease A, and lysozyme under conditions typical of HIC.

Keyword
Capillary, Column, HIC, Hydrophobic interaction chromatography, Monolith, Protein separation
Identifiers
urn:nbn:se:umu:diva-11762 (URN)doi:10.1002/jssc.200500239 (DOI)
Available from: 2007-04-23 Created: 2007-04-23 Last updated: 2009-09-17Bibliographically approved
2. Preparation of a Silica-based Sorbitol Methacrylate Grafted Stationary Phase for hydrophilic interaction chromatography
Open this publication in new window or tab >>Preparation of a Silica-based Sorbitol Methacrylate Grafted Stationary Phase for hydrophilic interaction chromatography
(English)Manuscript (Other (popular science, discussion, etc.))
Identifiers
urn:nbn:se:umu:diva-2545 (URN)
Available from: 2007-09-14 Created: 2007-09-14 Last updated: 2010-01-14Bibliographically approved
3. Atom-transfer radical graft polymerization initiated directly from silica applied to functionalization of stationary phases for high-performance liquid chromatography in the hydrophilic interaction chromatography mode.
Open this publication in new window or tab >>Atom-transfer radical graft polymerization initiated directly from silica applied to functionalization of stationary phases for high-performance liquid chromatography in the hydrophilic interaction chromatography mode.
2006 (English)In: Analytical Chemistry, ISSN 0003-2700, Vol. 78, no 20, 7098-7103 p.Article in journal (Refereed) Published
Abstract [en]

Initiation of atom-transfer radical polymerization of a number of monomers (styrene, methyl acrylate, 3-[N,N-dimethyl-N-(methacryloyloxyethyl)ammonium] propanesulfonate, butyl methacrylate, 2,3-epoxypropyl methacrylate) directly from chlorinated porous silica particles has been performed. The grafting has been confirmed and evaluated by Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. This initiation technique results in a hydrolytically stable initial Si-C bond, tethering the polymer to the silica substrate. The resulting grafted particles have been used as separation materials for both reversed-phase and hydrophilic interaction chromatography.

Identifiers
urn:nbn:se:umu:diva-11758 (URN)doi:10.1021/ac0602874 (DOI)
Available from: 2007-04-23 Created: 2007-04-23 Last updated: 2009-09-17Bibliographically approved
4. Evaluation of Alternative Organic Solvents for Hydrophilic Interaction
Open this publication in new window or tab >>Evaluation of Alternative Organic Solvents for Hydrophilic Interaction
In: Journal of Separation Science, ISSN 1615-9306Article in journal (Refereed) Submitted
Identifiers
urn:nbn:se:umu:diva-2547 (URN)
Available from: 2007-09-14 Created: 2007-09-14Bibliographically approved

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Hemström, Petrus

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