CuCo2O4 nanoparticle has been synthesized, characterized and firstly used as solid-phase extractant for the dispersive solid-phase extraction of Pb(II) in the presented work. The important parameters like pH of the working media, type of eluent solution and its volume, adsorbent amount, adsorption-desorption contact times, sample volume have been optimized. Lead (II) ions were quantitatively recovered on CuCo2O4 nanoparticle at pH 6.0 with 10 mg of adsorbent and eluted by using 2 mL of 1 M HCl. The influences of some cations and anions on the recoveries were also investigated. While the preconcentration factor was 25, the limit of detection was calculated as 6.5 mu g/L. The method was checked by applying the method to certified reference material (TMDA-53.3). The method was successfully applied to various food, cigarette and water samples.