There are different ways for antibiotics to enter the aquatic environment, with wastewater treatment plants (WWTP) considered to be one of the main points of entrance. Even treated wastewater effluent can contain antibiotics, since WWTP cannot eliminate the presence of antibiotics. Therefore, adsorption can be a sustainable option, compared to other tertiary treatments. In this direction, a versatile synthesis of poly(styrene-block-acrylic acid) diblock copolymer/Fe3O4 magnetic nanocomposite (abbreviated as P(St-b-AAc)/Fe3O4)) was achieved for environmental applications, and particularly for the removal of antibiotic compounds. For this reason, the synthesis of the P(St-b-AAc) diblock copolymer was conducted with a reversible addition fragmentation transfer (RAFT) method. Monodisperse superparamagnetic nanocomposite with carboxylic acid groups of acrylic acid was adsorbed on the surface of Fe3O4 nanoparticles. The nanocomposites were characterized with scanning electron microscopy (SEM), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM) analysis. Then, the nanoparticles were applied to remove ciprofloxacin (antibiotic drug compound) from aqueous solutions. The effects of various parameters, such as initial drug concentration, solution pH, adsorbent dosage, and contact time on the process were extensively studied. Operational parameters and their efficacy in the removal of Ciprofloxacin were studied. Kinetic and adsorption isothermal studies were also carried out. The maximum removal efficiency of ciprofloxacin (97.5%) was found at an initial concentration of 5 mg/L, pH 7, adsorbent’s dosage 2 mg/L, contact time equal to 37.5 min. The initial concentration of antibiotic and the dose of the adsorbent presented the highest impact on efficiency. The adsorption of ciprofloxacin was better fitted to Langmuir isotherm (R2 = 0.9995), while the kinetics were better fitted to second-order kinetic equation (R2 = 0.9973).