An effective extraction procedure based on the complexation of Cu2+, Cd2+, and Ni2+ with dithizone and extraction of these complexes by Tergitol NP-7 surfactant was developed. Micelle mediated extraction parameters such as pH, ligand and surfactant concentration, incubation time and temperature were investigated and optimized. Effects of external and internal interfering ions, linear dynamic range, detection and quantitation limits were examined and determined under optimal conditions. Detection limits were found as 0.5, 1.8 and 2.0 mg L-1 for Cu2+, Ni2+ and Cd2+, respectively. Linear dynamic range values were between 0.125-2, 0.125-2.5 and 0.05-1.4 μg mL-1 for Cu2+, Ni2+ and Cd2+ ions, respectively. Applicability, accuracy and precision of the method were checked with standard reference materials and real sample analyses by analyte addition technique. Finally, optimized method was applied to determine Cu2+, Ni2+ and Cd2+ contents of standard reference materials, mushrooms and water samples. Quantitative and accurate results were obtained from the analysis of standard reference materials and real samples.