The contamination of water bodies by pharmaceuticals, such as azithromycin (AZM), poses significant environmental concerns. In this study, electrospun polyacrylonitrile (PAN) reinforced with greenly synthesized iron oxide nanocomposite (PAN@Fe2O3) fibers sheet was prepared for the removal of azithromycin from water. The Fe2O3 nanopowder was synthesized via a facile and eco-friendly method using natural extracts as reducing and stabilizing agents. Then synthesized nanoparticles powder was incorporated in PAN surface by using simple electrospinning method. The morphology, structure, and composition of the nanocomposite fibers were characterized using XRD, FTIR, BET, FESEM and HRTEM analytical techniques. Utilising a molecular dynamics (MD) method, the mechanical characteristics of the PAN@Fe2O3 nanocomposite were theoretically examined. Batch adsorption experiments were conducted to evaluate the adsorption capacity of the nanocomposite fibers for AZM removal from aqueous solutions. The effects of various parameters such as dose, pH, contact time and initial AZM concentration on the adsorption process were investigated. The results demonstrated excellent adsorption performance, with a maximum adsorption capacity of 73.49 mg/g at pH=7. Furthermore, the adsorption kinetics and isotherms were analysed to understand the adsorption mechanism and equilibrium behaviour. Furthermore, for a minimum of four adsorption-desorption cycles, the adsorbent may be cycled and regenerate in succession.