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Thermoresponsive Poly(N-vinylcaprolactam) as Stationary Phase for Aqueous and Green Liquid Chromatography

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Abstract

Poly(N-vinylcaprolactam) (PVCL) connected to aminopropyl silica is a new stationary phase for temperature responsive liquid chromatography (TR-LC). PVCL shows a transition from hydrophilic to hydrophobic interaction between 30 and 40 °C. The synthesis is described in detail. The temperature responsive characteristic of the phase is illustrated with a mixture of steroids using pure water as mobile phase. An increase in retention is observed when raising the temperature. H–u plots at different temperatures were constructed. Below the lower critical solution temperature (LCST), no optimal velocity could be measured because of substantial resistance to mass transfer. Above the LCST, u opt was ca. 0.3 mm s−1 with reduced plate heights from 4 at 45 °C to 3 at 65 °C. The temperature responsive nature of the polymer is lost in green chromatography with ethanol as modifier in concentrations above 5%.

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Acknowledgement

Bram Miserez thanks the Institute for Encouragement of Innovation by Science and Technology Flanders for a study grant.

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Authors and Affiliations

  1. Pfizer Analytical Research Centre, Ghent University, Krijgslaan 281 S4-bis, 9000, Ghent, Belgium

    Bram Miserez, Frédéric Lynen & Pat Sandra

  2. Structural and Separation Sciences, Pfizer Global Research and Development, Ramsgate Road, Sandwich, Kent, CT13 9NJ, UK

    Adrian Wright

  3. Hichrom Ltd., 1 The Markham Centre, Station Road, Theale, Reading, Berkshire, RG7 4PE, UK

    Melvin Euerby

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  1. Bram Miserez
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  2. Frédéric Lynen
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  5. Pat Sandra
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Correspondence to Pat Sandra.

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Miserez, B., Lynen, F., Wright, A. et al. Thermoresponsive Poly(N-vinylcaprolactam) as Stationary Phase for Aqueous and Green Liquid Chromatography. Chroma 71, 1–6 (2010). https://doi.org/10.1365/s10337-009-1394-3

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  • DOI: https://doi.org/10.1365/s10337-009-1394-3

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