Magnetic nanofibrous composite membranes were electrospun from the mixtures of poly(acrylonitrile-co-acrylic acid) (PANCAA) and Fe(3)O(4) nanoparticles. Field emission scanning electron microscopy (FESEM) and thermal gravimetric analysis (TGA) were used to characterize the composite membranes. TGA results indicate that the addition of Fe(3)O(4) nanoparticles catalyzes the carbonization of PANCAA as well as dramatically increases the carbonization temperature. The intrinsic peroxidase-like activity of Fe(3)O(4) nanoparticles was measured by the color reaction of phenol/4-amino antipyrine in the presence of H(2)O(2). Under optimal conditions. the electrospun composite membranes show high peroxidase-like catalytic activity and reusability. Taking into account of the potentiality for separation. these as-prepared magnetic nanofibrous composite membranes will be applied in phenolic wastewater treatment. (C) 2009 Elsevier B.V. All rights reserved.