V(E) acetate-loaded methoxy poly(ethylene glycol)-b-poly(lactic acid) amphiphilic diblock copolymer nano-dispersion (PMV) was prepared by self-emulsification/solvent evaporation method. The drug-loaded amount, size distribution of PMV nanoparticles, and entrapment efficiency of V(E) acetate (V(E)A) were determined by UV and laser particle analyzer. Drug release in vitro was primarily investigated by UV. The results indicate that the size of PMV nanoparticles is less than 300 nm and PMV is largely influenced by preparation methods, property of solvents, V(E)A-fed amount, and the concentration of dispersion. The initial burst release is not observed and the accumulated release is more than 79% after 14 h. This study develops a new formulation for V(E)A and provides an experimental basis for the novel drug delivery systems of V(E)A.