During chemotherapy treatment, higher dosages of cancer drugs are more likely to affect the bone marrow; hence, several efforts must be used to diagnose cancers. We have synthesized nano-sized hydroxyapatite (nHAp) materials doped and co-doped with silver and iron by co-precipitation, yielding materials that can treat both the infections and malignant tumors. At higher Ag+/Fe2+ co-doping concentrations, an additional peak of iron oxide was obtained having morphologies spherical, rod-like, and flake-like structures. The nHAp and Ag+-HAp samples were diamagnetic, whereas the Fe2+-HAp and Ag+/Fe2+ co-doped samples were superparamagnetic. The in vitro 5-fluorouracil release profiles showed rapid drug release for Ag+-HAp, prolonged drug release for Fe2+-HAp and Ag+/Fe2+-HAp showed a pulsatile drug release. The in vitro biological toxicity study revealed that Ag+/Fe2+-HAp nanoparticles uptake in HeLa cells was more effective than in normal cells (HEK-293).