Matrix and core-shell doxorubicin-loaded nanoparticles were produced by single and coaxial electrospraying technique. The drug release and cytotoxicity assays of free DOX and nanoparticles are studied. The drug release from the nanoparticles was determined using a dialysis method,which is a common and recommended method for assessing drug release from nanoparticles. The cytotoxicity of free DOX, blank PLGA NPs, matrix DOX-loaded NPs and core-shell DOX-loaded NPs was measured by MTT assay. The raw data of the results are shown here.