Urchin-like NiCo2O4 hollow microspheres were synthesized by a solvothermal method and characterized by using X-ray diffraction, scanning electron microscopy, Brunauer-Emmett-Teller surface area, and zeta potential measurements. It was used as an adsorbent for the solid phase extraction of Pb(II) from water, food and street dust samples prior to its extraction with dilute HCl and its determination by FAAS. Figures of merit include a preconcentration factor of 30, a detection limit of 5.9 mu g L-1 and a relative standard deviation of 2.4%. The major advantage of the method is the fast equilibration during extraction without the need for vortexing or shaking. The method was successfully accurated by analyzing certified reference materials (BCR-482 Lichen, TMDA-70 Lake water and RM 8704 Buffalo River Sediment) and by analyzing spiked sea water, wastewater, well water, apple, eggplant, broccoli, ginger, lentil and street dust samples.