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Preparation and Evaluation of Long Chain Alkyl Methacrylate Monoliths for Capillary Chromatography

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Abstract

This work describes the fabrication of long chain alkyl methacrylate monolithic materials for use as stationary phases in capillary liquid chromatography. After capillary inner wall surface activation with 3-(trimethoxysilyl)propyl methacrylate, monoliths were formed by copolymerization of either lauryl or stearyl methacrylate (LMA or SMA) with ethylene dimethacrylate (EDMA) as crosslinker, in the presence of azobisisobutyronitrile (AIBN) as initiator and a mixture of porogenic solvents including water, 1-propanol and 1,4-butanediol. The composition of the polymerization mixture was changed in terms of monomer, crosslinker and porogen ratio composition, in order to compare the influence of these parameters. The monoliths were prepared in 320 μm i.d. and 200 mm length capillaries. The column morphology was characterized by optical microscopy and scanning electron microscopy (SEM). Total porosity and permeability of each column were calculated using uracil as unretained material by measuring the pressure drop across the columns as a function of linear velocity. The microglobule average size for each column was also determined using Hagen–Poiseuille equation and compared with the SEM images. As expected, a decrease of the porogen to monomer ratio corresponded to smaller microglobules and a lower total porosity. The columns were then chromatographically evaluated; good results were obtained when these capillaries were used to separate mixtures of phenols, aromatics and drug compounds.

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Acknowledgments

The Authors extend their appreciation to the Deanship of Scientific Research at King Saud University for funding the work through the Research Group No RGP-VPP-043.

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Authors and Affiliations

  1. Department of Chemistry, College of Science, King Saud University, P.O. Box 2455, Riyadh, 11451, Kingdom of Saudi Arabia

    Zeid A. ALOthman, Hadeel A. Al Abdelmoneim & A. Yacine Badjah-Hadj-Ahmed

  2. King Abdullah Institute for Nanotechnology, College of Science, King Saud University, P.O. Box 2454, Riyadh, 11451, Kingdom of Saudi Arabia

    Ahmad Aqel & Abdulrahman A. Al-Warthan

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  1. Zeid A. ALOthman
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  2. Ahmad Aqel
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  3. Hadeel A. Al Abdelmoneim
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  4. A. Yacine Badjah-Hadj-Ahmed
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  5. Abdulrahman A. Al-Warthan
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Correspondence to A. Yacine Badjah-Hadj-Ahmed.

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ALOthman, Z.A., Aqel, A., Al Abdelmoneim, H.A. et al. Preparation and Evaluation of Long Chain Alkyl Methacrylate Monoliths for Capillary Chromatography. Chromatographia 74, 1–8 (2011). https://doi.org/10.1007/s10337-011-2047-x

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  • DOI: https://doi.org/10.1007/s10337-011-2047-x

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