The increasing air pollution taking place in virtue of human activity has a novel impact in our health. Heterogeneous photocatalysis is a promising way of degrading volatile organic compounds (VOCs) that makes the quest of new and improved photocatalysts of great importance. Herein, perovskite-related materials ATiO3 with A = Mg, Ni, Co, Zn were synthesized through an ethylene glycol-mediated root, with ethylene glycol being used as a solvent and ligand. Characterization techniques such as X-ray diffraction (XRD), scanning electron microscopy, and energy dispersive X-ray spectroscopy (SEM/EDX), transmission electron microscopy (TEM), UV-vis spectroscopy, Raman spectroscopy, Fourier transform infrared (FT-IR), and photoluminescence spectroscopy (PL) were used in order to confirm the structure, the nanorod morphology, their absorption in UV-vis, and the separation efficiency of photogenerated charge carriers. The highest photoactivity was observed for ZnTiO3 in which 62% of toluene was decomposed after 60 min under LED illumination (54 mW/cm2).