A sensitive and simple method for the simultaneous preconcentration of trace amount Cu 2+ and Zn 2+ ions in some real samples has been established, which is based on the sorption of Cu 2+ and Zn 2+ on 3-((1H-indol-3-yl)-3,4,5-trimethyl)-1H-indole (ITMI) loaded on sodium dodecyl sulfate (SDS) coated alumina. The metal absorbed on the complexes was eluted using 3 mol/L nitric acid. The influences of the analytical parameters including pH and sample volume were investigated. The effects of matrix ions on the retentions of the analytes were also examined. The recoveries of analytes were generally higher than 95% with a low RSD. The method has been successfully applied to content evaluation of these metals in real samples.