Drug nanoparticles of water-insoluble bioactive compounds are potentially applicable in next-generation drug delivery systems (DDSs). As an example of such nanoparticles, the dimeric podophyllotoxin (PPT) was synthesized, and PPT nanoparticles were fabricated by the reprecipitation method. It was found that these nanoparticles show much higher cytotoxity for cancer cells as compared to etoposide, which is an analog of PPT.