Single-solidified floating organic drop microextraction was used for the preconcentration and determination of Cd(II) and Pb(II). The procedure employed 1-(2-pyridylazo)-2-naphthol as a chelating agent, 1-undecanol as the extractant solvent, and methanol as the dispersive solvent. Factors influencing the recovery of Cd(II) and Pb(II) such as the pH, volume of extractant, volume of ligand, volume of dispersant, and stirring time were optimized by Plackett Burman design. In order to complete the optimization, a central 2(3) +star orthogonal composite design was applied. The limits of detection for Cd(II) and Pb(II) were 0.15 and 0.52gL(-1). The validation of the procedure was evaluated by the analysis of TMDA 70 Fortified Water and NCSDC-73349 Bush Branches certified reference materials. The determined values were in good agreement with the certified values. The single-solidified floating organic drop microextraction method was employed for the determination of cadmium and lead in water, vegetables, and fruit.