Using a modified co-precipitation method, 11(2) nm γ-Fe2O3 nanoparticles functionalized with PSSNa [Poly(sodium 4-styrenesulfonate)] saloplastic polymer were successfully synthesized, and their structural, vibrational, electronic, thermal, colloidal, hyperfine, and magnetic properties were systematically studied using various analytic techniques. The results showed that the functionalized γ-Fe2O3/PSSNa nanohybrid has physicochemical properties that allow it to be applied in the magnetic remediation process of water. Before being applied as a nanoadsorbent in real water treatment, a short-term acute assay was developed and standardized using a Daphnia magna biomarker. The ecotoxicological tests indicated that the different concentrations of the functionalized nanohybrid may affect the mortality of the Daphnia magna population during the first 24 h of exposure. A lethal concentration of 533(5) mg L−1 was found. At high concentrations, morphological changes were also seen in the body, heart, and antenna. Therefore, these results suggested the presence of alterations in normal growth and swimming skills. The main changes observed in the D. magna features were basically caused by the PSSNa polymer due to its highly stable colloidal properties (zeta potential > −30 mV) that permit a direct and constant interaction with the Daphnia magna neonates.