A series of novel crosslinked polysucrose (PS) microspheres were prepared by a two-stage polymerization. A soluble (linear and/or comb) polysucrose was firstly synthesized by solution polymerization of sucrose and epichlorohydrin (EP); then the crosslinked polysucrose microspheres were prepared by reversed suspension polymerization of soluble PS with EP in chlorobenzene containing Span 80. The characterization by OM and SEM indicates that these spherical beads in diameters with the range from 250 to 450 mu m have smooth surface. The hydrated and dry densities, equilibrium water contents, and hydroxyl loadings of PS microspheres were investigated. The equilibrium water content values of these microspheres changed from 79.6% to 94.1%, and the hydroxyl contents were 15.5-19.0 m mol/g dependent on the cross-linking degrees. (c) 2006 Elsevier B.V. All rights reserved.