To　evaluate　the　potential　of　N-acetylated　chitosan　microspheres　used　as　a　chemoembolic　agent　in　vivo　and　in　vitro.　Calibrated　spherical　chitosan　microspheres　(CMs)　were　prepared　via　Water-in-Oil　emulsification　method　and　CMs　were　acetylated　(ACMs).　The　swelling　rate　of　CMs　was　greatly　affected　by　pH　than　that　of　ACMs　and　both　of　them　affected　by　temperature.　Microspheres　with　excellent　thermal　stability　demonstrated　controllable　degradation　in　lysozyme　solution.　Doxorubicin　was　released　from　microspheres　in　vitro　and　exhibited　excellent　control　release　profile.　ACMs　caused　hemolysis　less　than　CMs　(＜5%　of　the　time).　Co-culture　with　mouse　embryo　fibroblasts　revealed　that　microspheres　have　noncytotoxic　nature.　Microspheres　planted　in　a　rat　gluteal　muscle　demonstrated　that　it　were　biodegradable　and　biocompatible.　ACMs　were　performed　in　rabbit　ear　embolization　model　and　ischemic　necrosis　on　ear　was　visible　due　to　the　vascular　occlusion　after　15　days.　Acetylated　chitosan　microspheres　could　be　used　as　potential　biocompatible　and　biodegradable　embolic　agents.　(C)　2014　Published　by　Elsevier　Ltd.