Bovine serum albumin (BSA) nanoparticles containing arsenic trioxide (As(2)O(3)) were prepared by a pH-coacervation method. To investigate the properties of the As(2)O(3)-loaded BSA nanoparticles, a study on drug-to-polymer ratio was done to determine the drug loading (DL), and a H-600 transmission electron microscope (TEM) was used to examine the particle sizes. The results showed that the DL was 27.8% and the average particle size was about 734 nm. The drug release in vitro test was done, which revealed that the drug release was found to provide a slow release after an initial burst release and the cumulative percentage release reached close to 95%. In vitro cytotoxicity test was carried out using APL NB4 cell lines (acute promyelocytic leukemia), and the anticancer efficacy in vivo against mouse H22 hepatoma cells was evaluated on kungming mice. The results indicated that the anticancer efficacy of the As(2)O(3)-loaded BSA nanoparticles was very obvious.