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This work was intended to develop a new cross-linked gelatinized starch–xanthan gum hydrogel system, to characterize the properties of the new material, and to explore its potential applications in controlled drug delivery. Cross-linked starch–xanthan gum polymers were synthesized with varying levels of xanthan gum and sodium trimetaphosphate (STMP). The reaction of starch–xanthan gum polymers with STMP was examined using solid ³¹P NMR spectroscopy and FTIR. Morphology of the films made from the new polymers was studied by scanning electron microscopy. The swelling properties and the network parameters such as gel mesh size of the films were investigated. The permeation of solutes with various molecular weights and charges across the films was determined. ³¹P NMR and FTIR spectra showed that both starch and xanthan gum were reacted with STMP. The swelling ratio of the films was …