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Molecularly imprinted polymers grafted to flow through poly(trimethylolpropane trimethacrylate) monoliths for capillary-based solid-phase extraction
Umeå University, Faculty of Science and Technology, Department of Chemistry.
Umeå University, Faculty of Science and Technology, Department of Chemistry.
Umeå University, Faculty of Science and Technology, Department of Chemistry.
2006 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1109, no 1, 92-99 p.Article in journal (Refereed) Published
Abstract [en]

Monolithic previous termmolecularly imprinted polymersnext term (mMIPs) have been synthesized in a novel way using a trimethylolpropane trimethacrylate core material photo-polymerized in situ in a 100 μm I.D. UV-transparent capillary and further photo-previous termgraftednext term to create specific cavities in the previous termgraftednext term layer. This polymerization technique allows the imprints to be directly created on the surface of the material using a minimum amount of template. Three different anaesthetics of similar structures (bupivacaine, mepivacaine and S-ropivacaine) were used as model target molecules to synthesize sample enrichment media. Hence, various mMIPs have been prepared and evaluated on a micro-system against each analyte in order to test the retention properties and cross-selectivities of the materials. The retention factors were determined and compared with the non-previous termimprintednext term reference column (mNIP), yielding high imprinting factors together with good selectivity factors between the three analytes. A study with a pure enantiomeric target was carried out to assess the degree of stereo-specific imprinting for injection of racemic mixtures. Finally, one column was previous termimprintednext term with an equimolar mixture of all three anaesthetics to provide further comprehension of the retention mechanism and accredit the possibility of using the material as a sample enrichment entity. Scanning electron microscopy (SEM), nitrogen absorption/desorption (BET) and mercury intrusion porosimetry were used to characterize the monolith and the mMIPs properties. Nuclear magnetic resonance (NMR) has been used to assess the similarities between the mMIP and mNIP.

Place, publisher, year, edition, pages
Amsterdam: Elsevier , 2006. Vol. 1109, no 1, 92-99 p.
Keyword [en]
previous termMolecularly imprinted polymernext term, Bupivacaine, Monolith, Capillary, Liquid chromatography
URN: urn:nbn:se:umu:diva-12904DOI: doi:10.1016/j.chroma.2005.12.014OAI: diva2:152575
Available from: 2007-08-13 Created: 2007-08-13 Last updated: 2011-04-04Bibliographically approved
In thesis
1. Monolithic separation media synthesized in capillaries and their applications for molecularly imprinted networks
Open this publication in new window or tab >>Monolithic separation media synthesized in capillaries and their applications for molecularly imprinted networks
2006 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The thesis describes the synthesis of chromatographic media using several different approaches, their characterizations and applications in liquid chromatography. The steps to achieve a separation column for a specific analyte are presented. The main focus of the study was the design of novel molecularly imprinted polymers.

Attachment of monolithic polymeric substrates to the walls of fused silica capillaries was studied in Paper I. With a broad literature survey, a set of common methods were tested by four techniques and ranked by their ability to improve anchoring of polymers. The best procedure was thus used for all further studies.

Synthesis of monoliths in capillary columns was studied in Paper II. With the goal of separating proteins without denaturation, various monoliths were polymerized in situ using a set of common monomers and cross-linkers mixed with poly(ethylene glycol) as porogen. The resulting network was expected to present “protein-friendly pores”. Chemometrics were used to find and describe a set of co-porogens added to the polymerization cocktails in order to get good porosity and flow-through properties.

Assessment of the macroporous structure of a monolith was described in Paper III. An alternative method to mercury intrusion porosimetry was proposed. The capillaries were embedded in a stained resin and observed under transmission electron microscope. Images were then computed to determine the pore sizes.

Synthesis of molecularly imprinted polymers grafted to a core mono-lith in a capillary was described in Paper IV. The resulting material, imprinted with local anaesthetics, was tested for its chromatographic performance. Similar imprinted polymers were characterized by microcalorimetry in Paper V. Finally, imprinted monoliths were also synthesized in a glass tube and further introduced in a NMR rotor to describe the interactions between stationary phase and template in Paper VI.

Place, publisher, year, edition, pages
Umeå: Kemi, 2006. 50 p.
bupivacaine, etching, phosphorylated tyrosine, poly(ethylene glycol), silanization, transmission electron microscopy, fused silica capillaries, isothermal titration calorimetry, local anæsthetic, molecularly imprinted polymer, monolith, nuclear magnetic resonance
National Category
Analytical Chemistry
urn:nbn:se:umu:diva-923 (URN)91-7264-207-6 (ISBN)
Public defence
2006-12-01, Lilla Hörsallen KB3A9, KBC-Huset, Umeå University, Umeå, Sweden, 10:00
Available from: 2006-11-10 Created: 2006-11-10 Last updated: 2011-04-15Bibliographically approved

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