Electrospinning and photocrosslinking were combined in this Study to prepare water-insoluble fibers of polyvinyl alcohol (PVA) with the styrylpyridinium (SbQ) pendent group. The PVA-SbQ exhibited high photosensitivity in a spectroscopic study. Electrospun PVA and PVA-SbQ fibers were soluble and totally dissolved after water immersion. UV irradiation of the electrospun mat led to a significant decrease in the mass loss of PVA-SbQ fibers in water. This water insolubility was confirmed by the stable morphology of PVA-SbQ fibers during water immersion. (C) 2008 Elsevier B.V. All rights reserved.