A two-step doping strategy was applied to the synthesis of La0.9Sr0.1Ga0.8Mg0.2O2.85(LSGM1020) powder by a gel combustion method. The Mg-doped LaGaO3 powder was prepared in the first step, and Sr incorporation in the Mg-doped LaGaO3 powder was done in the second step to obtain the final LSGM1020 powder. The two-step procedure is effective in preparing higher purity powders than the traditional one-step procedure. Rietveld refinement of X-ray powder diffraction (XRD) patterns shows that incorporation of Mg in LaGaO3 in the first step enlarges the LaGaO3 lattice: this facilitates the incorporation of Sr in the second doping step and thus high purity powder is obtained. Relatively phase pure LSGM1020 powder with only 3.1% of LaSrGaO4 was obtained after calcination at 1300 degrees C for 5 h. Therefore, the two-step doping strategy is an effective procedure for the preparation of LSGM powders with high Sr- and Mg-doping levels.