Thermoresponsive poly(N-vinylcaprolactam) as stationary phase for aqueous and green liquid chromatography

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 degrees 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 degrees C to 3 at 65 degrees C. The temperature responsive nature of the polymer is lost in green chromatography with ethanol as modifier in concentrations above 5%