Transition metals such as V, Fe, and Ni were used to synthesize doped zinc oxide nanoparticles from mixed liquid precursors by using the flame spray pyrolysis (FSP). The effects of dopants on the powder properties such as morphology, specific surface area, crystal structure, and light adsorption were analyzed by TEM, BET, XRD, and UV-Vis diffuse reflection spectrum (DRS), respectively. The results showed that hexagonal wurtzite structured ZnO:M (M = V, Fe, Ni) nanoparticles were successfully synthesized by the FSP. The transition metal-doping resulted in the decrease in its particle size and crystallite size. The UV-vis absorption spectra of ZnO:M nanoparticles were also red-shifted. ZnO:V showed the highest MB degradation of 99.4% under the UV irradiation after 3 hrs.