Chemoembolization based on microspheres have been emerged as a novel and promising way for interventional therapy, however, the exact effect and probable mechanism have not been revealed. The purpose of our study was to evaluate the potential of Pingyangmycin loaded bovine serum albumin microspheres (PYM-BSA-MSs) for chemoembolization therapy both in vitro and in vivo. The effect of PYM-BSA-MSs on cell growth curves and changes of cell morphology and activities measured by MTT assay were carried out in human umbilical vein endothelial ECV-304 cells. The in vivo occlusion effect was evaluated in 24 healthy rabbits. Macroscopic examinations and Hematoxylin-Eosin (H-E) staining of cross-section of rabbits' central auricular arteries were employed to observe the apparent and histological changes of arterioles. The results show that the PYM-BSA-MSs could inhibit the proliferation and induce the apoptosis of ECV-304 cells in a time-dependent manner. In vivo studies demonstrated that 21 days after artery embolization with the PYM-BSA-MSs, neointimal thickening of arterioles and significant hyperplasia of endothelial cells could be detected, but without completely interruption of blood flow. Compared with plain PYM aqueous solution or BSA-MSs oily suspension, PYM-BSA-MSs showed excellent potential as an alternative to interventional embolization materials.