Semiconductor photocatalysts, particularly ZnO nanoparticles, were synthesized via the precipitation method using four different precursors (zinc acetate/zinc nitrate/zinc sulfate/zinc chloride) and compared, according to their optical, structural, photocatalytic, and anticancer properties. The materials were characterized via X-ray Diffraction method (XRD), micro-Raman, Fourier Transform Infrared Spectroscopy (FT-IR), Brunauer–Emmett–Teller (BET), Dynamic Light Scattering (DLS), and Field Emission Scanning Electron Microscope (FESEM) analysis. Photocatalysis was conducted under UV and visible light irradiation, using Rhodamine B as the organic pollutant. It was observed that the highest photocatalysis efficiency was obtained by the nanoparticles synthesized from the zinc acetate used as precursor material. A cell-dependent anticancer efficiency of the tested ZnO nanoparticles was also observed, that was also attributed to the different precursors and the synthesis method, revealing that the nanoparticles that were synthesized from zinc acetate were more bioactive among the four tested precursors. Overall, the data revealed that both the enhanced photocatalytic and biological activity of ZnO nanoparticles derived from zinc acetate precursor could be attributed to the reduced crystalline size, increased surface area, as well as the observed hexagonal crystalline morphology.