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Preparation and evaluation of monolithic poly(N-vinylcarbazole-co-1,4-divinylbenzene) capillary columns for the separation of small molecules

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Abstract

Short-term polymerization or the so-called low-conversion polymerization was applied for the preparation of N-vinylcarbazole (NVC) and 1,4-divinylbenzene (DVB) monolithic capillary columns. The synthesis was carried out by thermally initiated free radical copolymerization under the influence of inert micro- (toluene) and macroporogen (1-decanol) and α,α′-azoisobutyronitrile (AIBN) as radical initiator. The morphological and porous properties were studied by scanning electron microscopy (SEM), nitrogen adsorption, and mercury intrusion porosimetry (MIP). The copolymerization process was studied by monomer conversion measurements. This approach led to increased porosity and specific surface area. A specific surface area above 400 m2/g of the monolith and a distinct bimodal pore size distribution were obtained. The chromatographic performance was determined in terms of theoretical plate heights and number of theoretical plates. The lowest plate height value was found to be 3.9 μm (corresponding to ≈256,000 plates per meter) applying methylparaben utilizing an 80 mm × 0.2 mm i.d. monolithic capillary. The developed NVC/DVB monolithic supports showed high separation efficiency towards small molecules, which was exemplified applying reversed-phase (RP) separation of alkylbenzenes, beta-blockers, flavanoids, parabens, and phenones. The loading capacity was analyzed for isocratic separation of seven alkylbenzenes and was found to be up to 77 ng total mass of alkylbenzenes. Furthermore, a long-term stability test of 1,000 consecutive runs was performed and resulted in a maximum variance of 0.97, 0.85, and 0.16 % RSD for resolution, peak width at half height, and retention times, respectively. The material was proven to have a high permeability of 1.11E−14 m2, applying water as a mobile phase.

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Acknowledgments

The authors thank the Genome Research in Austria (GEN-AU) (Federal Ministry for Education, Science and Culture, Vienna, Austria) and SFB021 for financial support of the presented work. The authors would like to thank Thomas Bielz (Institute of Physical Chemistry, University of Innsbruck) for his support in interpreting nitrogen sorption data.

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Authors and Affiliations

  1. Institute of Analytical Chemistry and Radiochemistry, Leopold-Franzens University, Innrain 80-82, 6020, Innsbruck, Austria

    Rainer Koeck, Martin Fischnaller, Rania Bakry & Guenther K. Bonn

  2. Institute of Mineralogy and Petrography, Leopold-Franzens University, Innrain 52, 6020, Innsbruck, Austria

    Richard Tessadri

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  1. Rainer Koeck
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  2. Martin Fischnaller
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  3. Rania Bakry
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  5. Guenther K. Bonn
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Correspondence to Rania Bakry.

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Koeck, R., Fischnaller, M., Bakry, R. et al. Preparation and evaluation of monolithic poly(N-vinylcarbazole-co-1,4-divinylbenzene) capillary columns for the separation of small molecules. Anal Bioanal Chem 406, 5897–5907 (2014). https://doi.org/10.1007/s00216-014-8007-1

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  • DOI: https://doi.org/10.1007/s00216-014-8007-1

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