Recebido em 21/3/13; aceito em 16/5/13; publicado na web em 25/7/13 A simple and fast approach for solid phase extraction is herein described, and used to determine trace amounts of Pb 2+ and Cu 2+ metal ions. The solid phase support is sodium dodecyl sulfate (SDS)-coated γ-alumina modified with bis(2-hydroxy acetophenone)-1,6-hexanediimine (BHAH) ligand. The adsorbed ions were stripped from the solid phase by 6 mL of 4 M nitric acid as eluent. The eluting solution was analyzed by flame atomic absorption spectrometry (FAAS). The sorption recovery of metal ions was investigated with regard to the effects of pH, amount of ligand, γ-alumina and surfactant and the amount and type of eluent. Complexation of BHAH with Pb 2+ or Cu 2+ ions was examined via spectrophotometry using the HypSpec program. The detection limit for Cu 2+ was 7.9 µg L -1 with a relative standard deviation of 1.67%, while that for Pb 2+ was 6.4 µg L -1 with a relative standard deviation of 1.64%. A preconcentration factor of 100 was achieved for these ions. The method was successfully applied to determine analyte concentrations in samples of liver, parsley, cabbage, and water.