LaSrFeCoO₆ was prepared by sol-gel method with different complexing agents (citric acid, tartaric acid, glucose, sucrose, EDTA). The title catalysts were characterized by XRD, BET, H2-TPR, TG-DSC and SEM techniques. The catalytic activity was evaluated for methane combustion. In the experiment different agents were used to prepare catalyst, which was calcined at 800 ℃ for three hours. The obtained catalyst has complete perovskite crystal. Different complexing agents have great influence on the structure and properties of the catalyst. When citric acid was used as the complexing agent, the LaSrFeCO₆ catalyst had better catalytic activity; the conversion of 10% and 90% was obtained at 425 ℃ and 600 ℃, respectively.