Perovskite (ABO3) and quasi-perovskite brownmillerite (A2B2O5) compounds (BaFeO3, Sr2Fe2O5, Ca2Fe2O5, BaCoO2.93, Sr2Co2O5) were prepared by the citrate-nitrate combustion method. The compounds were measured by X-ray diffraction, ultravio- let-visible spectrophotometry, Fourier transform infrared spectroscopy and scanning electron microscopy. The calcination tempera- ture of the samples was maintained at 450 ℃ for 2 h and 800 ℃ for 4 h. Experiments prove that the synthesized samples are in- clined to form perovskite with larger ion radius of A-site elements when the B-site element was fixed. Synthesized perovskites and brownmillerites have certain photocatalysis properties.