The features of microparticles, as size, surface structure, and morphology, depend, mainly, on the methodology used for their preparation. Emulsion polymerization techniques are undoubtedly among the most widespread. However, the use of toxic, volatile organic solvents represents a major disadvantage, namely, because of environmental issues. In this study, we prepared glutaraldehyde crosslinked chitosan-poly(vinyl alcohol) microparticles by an improved water-in-oil emulsion technique using corn oil as organic phase. The application of this polymeric blend as microparticle is scarcely investigated. As resulting of the procedure here presented, spherical and smooth surface microparticles were obtained, with mean diameter of 16 lm. The cross-linking reaction between the aldehyde and the amino or the hydroxyl groups formed either an imine (Schiff's base) or an acetal bond, respectively, as analyzed by infrared spectroscopy. The microparticles here described did not present cytotoxic potential. Accordingly, this study can find promising and successful application in biotechnology.