In this study, a new magnetic solid phase extraction method (MSPE) was developed for the enrichment and separation of trace amount Pb(II) on the magnetic nanoparticles synthesized using lemon peel (Fe3O4-LP). The determination of Pb(II) in the samples was performed with inductively coupled plasma mass spectrometry. The Fe3O4-LP was characterized by scanning electron microscopy, X-ray powder diffractometry, Brunauer-Emmett-Teller surface area analysis, and vibration sample magnetometry. The effect of different parameters such as pH, adsorption and elution time, concentration of eluent and volume and matrix effect on the recovery of Pb(II) was investigated for the MSPE. Considering preconcentration factor, the detection limit value of the proposed method was calculated to be 39 ng/L for Pb (II). The accuracy of the developed method was tested with analysis of the BCR 185 R Bovine Liver and 2976a Mussel Tissue certified reference materials. The results were in good agreement with the certified values.