Hydrogel hybrids were conveniently prepared from alkaline hydrolysis of chitosan-poly(acrylonitrile) mixture under highly practical conditions. The reaction of chitosan alkoxide anions with nitrile groups of poly(acrylonitrile) (PAN) forms crosslinking points and results in a three-dimensional network with superswelling ability in aqueous media. The hydrogel hybrid was identified using FTIR spectroscopy. The PAN content of the hydrolyzing feed affects proportionally the swelling capacity of the hydrogel hybrid. The swelling properties (capacity and rate) of the ampholytic hydrogel were investigated preliminarily. (c) 2005 Wiley Periodicals, Inc.