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Organo-silica hybrid capillary monolithic column with mesoporous silica particles for separation of small aromatic molecules

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Abstract

Monolithic stationary phases for use in capillary electrochromatography were prepared by incorporation of mesoporous silica particles (of type MCM-41 or UVM-7) in a polymer obtained from butyl methacrylate and ethylene glycol dimethacrylate as monomers, 1,4-butanediol and 1-propanol as porogen, and azobisisobutyronitrile as initiator. The stability of the dispersions with varying fractions of silica particles was investigated by UV-vis spectrometry. Using continuous stirring during the capillary filling and short UV-polymerization times, polymeric beds with homogenously dispersed mesoporous particles (with contents up to 35 wt% of silica) are obtained. The resulting hybrid monolithic columns were characterized using scanning electron microscopy. The chromatographic performance of these novel stationary phases was evaluated by using alkyl benzenes and benzoic acid derivatives as test analytes. The use of these polymers leads to increased retention and separation efficiency compared to the parent monolith. The column efficiency reached values of up to 140,000 plates m−1. The resulting hybrid monolithic columns also exhibited a satisfactory reproducibility with relative standard deviations of ca. 14% (batch-to-batch).

Hybrid polymer monoliths containing large amounts of mesoporous silica-particles (MCM-41 or UVM-7) were prepared by UV initiation. The prepared monolithic columns showed higher retention times and efficiencies than parent monoliths for alkyl benzenes and benzoic acid derivatives.

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Acknowledgements

This work was supported by projects CTQ2014-52765-R and MAT2015-64139-C4-2-R (MINECO of Spain and Fondo Europeo de Desarrollo Regional, FEDER) and PROMETEO/2016/145 (Conselleria d’Educació, Investigació, Cultura i Esport, Generalitat Valenciana, Spain).

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Authors and Affiliations

  1. Department of Analytical Chemistry, University of Valencia, Dr. Moliner 50, 46100, Burjassot, Valencia, Spain

    Anica Weller, Enrique Javier Carrasco-Correa, Carolina Belenguer-Sapiña, Adela de los Reyes Mauri-Aucejo & José Manuel Herrero-Martínez

  2. University of Valencia, Institut de Ciència dels Materials, P.O. Box 22085, 46071, Valencia, Spain

    Pedro Amorós

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  1. Anica Weller
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  2. Enrique Javier Carrasco-Correa
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  3. Carolina Belenguer-Sapiña
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  6. José Manuel Herrero-Martínez
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Correspondence to José Manuel Herrero-Martínez.

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Weller, A., Carrasco-Correa, E.J., Belenguer-Sapiña, C. et al. Organo-silica hybrid capillary monolithic column with mesoporous silica particles for separation of small aromatic molecules. Microchim Acta 184, 3799–3808 (2017). https://doi.org/10.1007/s00604-017-2404-z

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  • DOI: https://doi.org/10.1007/s00604-017-2404-z

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