Glutaraldehyde was used as a crosslinking reagent to produce electrospun zein fibers with improved physical properties and solvent resistance. Using 8% glutaraldehyde, round and ribbon fibers were produced with diameters between 1 and 70 mu m. All fibers readily dissolved in acetic acid. Heating the zein/glutaraldehyde fibers at temperatures from 80 to 180 degrees C for different times provided various degrees of insolubility to the fibers. A model was developed relating the extent of dissolution with the amount of glutaraldehyde used and the temperature/time at which the fiber was exposed. The fibers were found to be birefringent; upon heating, the amount of alpha-helix in the fiber was reduced.