Sepabeads SP70 resin was impregnated with ionic liquid (BMIMPF6) was used for micro-solid phase extraction of lead(II) prior to its microsampling flame atomic absorption spectrometric determination. The optimum values of experimental parameters such as adsorbent amount, ligand amount, pH, eluent type and concentration, eluent volume, sample volume on recovery of lead were optimized as 5.0 mg, 0.15 mg, 7, HCl, 2 M, 0.4 mL, 50 mL, respectively. The analytical data of the method under optimal condition are as follows; limit of detection (LOD) (3 s/m, N: 10): 0.21 μg L−1, limit of quantification (LOQ) (10 s/m, N: 10): 0.69 μg L−1, preconcentration factor (PF): 125, and relative standard deviation (RSD%): 1.43%. The accuracy of the developed method was checked by addition-recovery tests to real samples and analysis of certified reference materials (Environment Canada TMDA-53.3 (fortified water) and 1570a trace elements in spinach leaves). The recovery values of these analyses are in the range of 90–98%. The method was successfully applied to determination of lead level of food and water samples.