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Visible light initiated polymerization of styrenic monolithic stationary phases using 470 nm light emitting diode arrays

Authors

  • Zarah Walsh,

    1. Irish Separation Science Cluster, National Centre for Sensor Research and School of Chemical Sciences, Dublin City University, Glasnevin, Dublin, Ireland
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  • Pavel A. Levkin,

    1. The Molecular Foundry, E.O. Lawrence Berkeley National Laboratory, Berkeley, CA, USA
    Current affiliation:
    1. Forschungszentrum Karlsruhe and Heidelberg University, Germany
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  • Vijay Jain,

    1. The Molecular Foundry, E.O. Lawrence Berkeley National Laboratory, Berkeley, CA, USA
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  • Brett Paull,

    1. Irish Separation Science Cluster, National Centre for Sensor Research and School of Chemical Sciences, Dublin City University, Glasnevin, Dublin, Ireland
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  • Frantisek Svec,

    1. The Molecular Foundry, E.O. Lawrence Berkeley National Laboratory, Berkeley, CA, USA
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  • Mirek Macka

    Corresponding author
    1. Irish Separation Science Cluster, National Centre for Sensor Research and School of Chemical Sciences, Dublin City University, Glasnevin, Dublin, Ireland
    • School of Chemical Sciences, Dublin City University, Glasnevin, Dublin 9, Ireland Fax: +353-1-700-5503
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Abstract

Poly(styrene-co-divinylbenzene) monolithic stationary phases have been synthesized for the first time by photoinitiated polymerization. An initiator composed of (+)-(S)-camphorquinone/ethyl-4-dimethylaminobenzoate/N-methoxy-4-phenylpyridinium tetrafluoroborate was activated using a 470 nm light emitting diode array as the light source. Spatially controlled polymerization of styrenic monoliths has been achieved within specific sections of a 100 μm id polytetrafluoroethylene-coated fused-silica capillary using simple photo masking. The sharpness of the edges was confirmed by optical microscopy, while SEM was used to verify a typical porous, globular morphology. Flow resistance data were used to assess the permeability of the monoliths and they were found to have good flow through properties with a flow resistance of 0.725 MPa/cm at 1 μL/min (water, 20°C). Conductivity profiling along the length of the capillary was used to assess their lateral homogeneity. Monoliths which were axially rotated during polymerization were found to be homogeneous along the whole length of the capillary. The monolithic stationary phases were applied to the RP gradient separation of a mixture of proteins. Column fabrication showed excellent reproducibility with the retention factor (k) having a RSD value of 2.6% for the batch and less than 1.73% on individual columns.

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