This paper presents structural, morphological and preliminary ultrasonic characterizations of the β-Cyclodextrin/hydroxyapatite (CD-HAp) composites synthesized by an adapted co-precipitation method. The structural and morphological properties were evaluated by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDX). The specific surface area, pore size and pore volume were determined using the methods of Brunauer–Emmett–Teller (BET) and Barrett–Joyner–Halenda (BJH), respectively. The novelty of our study consists in preliminary ultrasonic measurements conducted on CD-HAp composite, uniformly dispersed in distilled water. The benefit of this non-destructive method was to facilitate and simplify the characterization techniques of nanoparticles. Our experiments proved that the efficiency of lead ion removal by CD-HAp composites depended on the initial concentration of lead. The maximum adsorption capacity of the solid phase, for Pb2+ indicated a higher rate of removal by the CD-HAp_2. These adsorption results bring valuable insight into the beneficial contribution of our compounds, for the removal of heavy metal ions from aqueous solutions. Furthermore, in the present study, was evaluated the toxic effect of lead ions adsorbed by hydroxyapatite from contaminated water on HeLa cells.