A novel solid phase extraction procedure for determination of copper, lead and iron in natural water and food samples has been established in the presented work. 1-Phenylthiosemicarbazide (1-PTSC) as ligand and Dowex Optipore L-493 resin as adsorbent were used in a mini chromatographic column. Various analytical conditions for the quantitative recoveries of analyte ions including pH, amounts of adsorbent, eluent, sample volume, etc. were investigated. The recovery values for analyte ions were higher than 95%. The determination of copper, lead and iron was performed by flame atomic absorption spectrometry. The influences of some alkali, alkali earth and transition metals on the recoveries of analyte ions were investigated. The preconcentration factor was 62.5. The limit of detections of the understudied analytes (k = 3, N = 21) were 0.64 mu g L-1 for copper, 0.55 mu g L-1 for lead and 0.82 mu g L-1 for iron. The relative standard deviation was found to be lower than 6%. The accuracy of the method was confirmed with certified reference material (GBW 07605 Tea). The method was successively applied for the determination of copper, lead and iron in water and some food samples including cheese, bread, baby food, pekmez, honey, milk and red wine after microwave digestion. (C) 2010 Elsevier Ltd. All rights reserved.