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Synthesis and Evaluation of Polymer-Based Zwitterionic Stationary Phases for Separation of Ionic Species
Umeå University, Faculty of Science and Technology, Department of Chemistry.
Umeå University, Faculty of Science and Technology, Department of Chemistry.
2001 (English)In: Analytical Chemistry, ISSN 0003-2700, E-ISSN 1520-6882, Vol. 73, no 9, 1993-2003 p.Article in journal (Refereed) Published
Abstract [en]

Three different zwitterionic functional stationary phases for chromatography were synthesized on the basis of 2-hydroxyethyl methacrylate (HEMA) polymeric particles. Two synthesis routes, producing materials designated S300-ECH-DMA-PS or S300-TC-DMA-PS, involved activation of the hydroxyl groups of the HEMA material with epichlorohydrin or thionyl chloride, respectively, followed by dimethylamination and quaternizing 3-sulfopropylation with 1,3-propane sultone. The third route was accomplished by attaching methacrylate moieties to the HEMA through a reaction with methacrylic anhydride, followed by graft photopolymerization of the zwitterionic monomer 3-[N,N-dimethyl-N-(methacryloyloxyethyl)ammonium] propanesulfonate, initiated by benzoin methyl ether under 365-nm light. According to elemental analyses, both the S300-ECH-DMA-PS and S300-TC-DMA-PS materials appeared to have overall charge stoichometries close to unity, whereas the grafted material, S300-MAA-SPE, seemed to carry an excess of anion exchange sites in addition to the zwitterionic groups. Yet all three zwitterionic stationary phases were capable of separating inorganic anions and cations simultaneously and independently using aqueous solutions of perchloric acid or perchlorate salts as eluent, albeit with markedly different selectivities. On the S300-TC-DMA-PS and S300-MAA-SPE materials, the retention times increased for cations and decreased for anions with increasing eluent concentration, whereas with the S300-ECH-DMA-PS material, the retention times of both anions and cations decreased with increasing eluent concentration. These results demonstrate the importance of choosing appropriate synthesis conditions in order to prepare covalently bonded zwitterionic separation materials with an acceptable charge balance.

Place, publisher, year, edition, pages
American Chemical Society (ACS), 2001. Vol. 73, no 9, 1993-2003 p.
National Category
Chemical Sciences
Identifiers
URN: urn:nbn:se:umu:diva-2937DOI: 10.1021/ac000933dOAI: oai:DiVA.org:umu-2937DiVA: diva2:141308
Available from: 2003-11-14 Created: 2003-11-14 Last updated: 2012-06-04Bibliographically approved
In thesis
1. Zwitterionic Separation Materials for Liquid Chromatography and Capillary Electrophoresis: Synthesis, Characterization and Application for Inorganic Ion and Biomolecule Separations
Open this publication in new window or tab >>Zwitterionic Separation Materials for Liquid Chromatography and Capillary Electrophoresis: Synthesis, Characterization and Application for Inorganic Ion and Biomolecule Separations
2003 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Liquid Chromatography (LC) and Capillary Electrophoresis (CE) are modern analytical techniques that play very important roles in many areas of modern science such as life science, biotechnology, biomedicine, environmental studies, and development of pharmaceutics. Even though these two techniques have existed and been subjected to studies for several decades, the developments of new separation materials for them are still very important till now in order to meet the different new demands for improvement from other disciplines in science.

In this doctoral thesis, several novel covalently bonded sulfobetaine type zwitterionic separation materials are synthesized for the application in LC and CE. These materials carry both positively charged quaternary ammonium groups and negatively charged sulfonic groups, which result in a very low net surface charge compared to conventional separation materials with only anionic or cationic functional groups. Consequently, it is possible to employ these materials for separation of different ionic species under mild conditions. The surface properties have also been characterized, mainly by elemental analysis, sorption isotherm, ζ-potential measurements, and spectroscopic methods.

By using packed zwitterionic columns for liquid chromatography, small inorganic anions or cations, and acidic or basic proteins can be independently and simultaneously separated in a single run using optimal sets of separation conditions. This is a unique property compared to conventional ionic separation material for LC. When fused silica capillaries coated with zwitterionic polymer are used for capillary electrophoresis, good separations can be achieved for solutes as different as inorganic anions, peptides, proteins, and tryptically digested proteins.

Publisher
53 p.
Keyword
Analytical chemistry, Zwitterionic, stationary phase, separation, liquid chromatography, capillary electrophoresis, sulfobetaine, modification, covalently bonded, graft polymerization, ζ-potential, Analytisk kemi
National Category
Analytical Chemistry
Identifiers
urn:nbn:se:umu:diva-153 (URN)91-7305-543-3 (ISBN)
Public defence
2003-12-05, Umeå, 10:00
Available from: 2003-11-14 Created: 2003-11-14Bibliographically approved

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Irgum, Knut

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