Abstract: The calibration curve was prepared by the matrix matching method and La was used as the internal standard for calibration to eliminate the influence of matrix effect and instrument drift. The determination method of Al, Mg contents in zinc-aluminum-magnesium alloy by inductively coupled plasma optical emission spectrometry (ICP-OES) was set up. The method was applied to the determination of zinc-aluminum-magnesium alloy sample, the relatively standard deviations were between 0.86% and 2.13%, and the recoveries were between 96.4% and 99.6%. Compared with the chemical analysis method, the results were in good agreement.