A composite material prepared by polymerization of β-cyclodextrin (β-CD) on the surface of natural hydroxyapatite using citric acid as cross linker, was employed as electrode material for the detection of Pb(II). Hydroxyapatite was obtained from bovine bones, following a three-step procedure including precalcination, chemical treatment with (NH 4 ) 2 HPO 4 and calcination. The structure of the pristine hydroxyapatite (NHAP P0.5 ) and its functionalized counterpart (NHAP p0.5 -CA-β-CD) materials was examined using XRD and FTIR. Upon deposition as thin lm on a glassy carbon electrode (GCE), the ion exchange ability of NHAP p0.5 -CA-β-CD was exploited to elaborate a sensitive sensor for the detection of lead. The electroanalytical procedure was based on the chemical accumulation of lead ions under opencircuit conditions, followed by the detection of the preconcentrated species using differential pulse anodic stripping voltammetry. The reproducibility of the proposed method based on different measurements in a solution containing 2 µM lead gave a coe cient of variation of 1.27%. Signi cant parameters that can affect the lead stripping response were optimized: a linear calibration curve for lead (II) in the concentration range of 2 × 10 − 8 mol L − 1 − 20 × 10 − 8 mol L − 1 (R 2 = 0.998) was obtained. The detection limit (DL = 3S/M) and the sensitivity of the proposed sensor were 5.06 × 10 − 10 mol L − 1 and 100.80 µA.µM − 1 , respectively. The interfering effect of several ions expected to affect the stripping determination of lead was evaluated, and the proposed sensor was also successfully applied in the determination of Pb 2+ ions in spring water and well water.