Communication: Segmented polymer networks containing poly(methyl vinyl ether) (PMVE) segments were prepared by free-radical-initiated copolymerization of PMVE-alpha,omega-dimethacrylate with styrene or 2-hydroxyethyl methacrylate (HEMA). These networks were evaluated as thermo-responsive solid-phase extraction materials. Suspension-derived polymer networks consisting of 80% of PMVE and 20% of HEMA adsorb toluene from an aqueous solution at 40degreesC and release the adsorbed toluene quantitatively at 20degreesC.