Hepatocellular carcinoma (HCC) might be efficiently treated using drug-eluting beads (DEB) combined with transarterial chemo-embolization (TACE) which showed improved survival of patients. DEB-TACE, as a novel locoregional treatment for HCC, allows loading of pre-calibrated beads with either an anticancer agent – such as doxorubicin (DOX). The combination of embolic beads with a multi-targeted tyrosine kinase inhibitor that inhibits tumor vessel growth is also suggested as an alternative, such as Sunitinib (SUN), an inhibitor of VEGFRs and other receptor tyrosine kinases implicated in HCC angiogenesis. Current marketed products are nondegradable drug-free beads. Physicians would like to have biodegradable beads to allow multiple interventions on the patient if needed. This work aims to develop and characterize biodegradable microspheres that adhere to most of the needed features of embolic beads, and to study their loading and release profiles of selected anticancer and anti-angiogenic drugs.