A series of novel hydrogel polysucrose microspheres with the mean size ranging from 200 to 500 pm were prepared via two-step method. First, soluble polysucrose was synthesized by solution polymerization between sucrose and epichlorohydrin; second, a reversed phase suspension crosslinking reaction was performed to prepare polysucrose microspheres. The SEM images indicated that these spherical beads had smooth surface and hydrogel interior structure. FTIR was used to characterize the chemical structure of the beads. The hydrated and dry densities, equilibrium water content, and hydroxyl content of polysucrose microspheres were also investigated. The characteristic of high hydroxyl content (15.48-19.04 mmol/g) make these microspheres suitable for protein adsorption. Meanwhile, bovine serum albumin was used to examine the adsorption capacity of the microspheres. These microspheres had a capacity as high as 49.28 mg/g. The adsorption kinetics and recycling of the beads were also investigated. (c) 2006 Wiley Periodicals, Inc.