In this project, a prompt, efficient, and effective method for Cd²⁺ ions extraction from different food and water samples using magnetic dispersion-based solid phase extraction by functionalized iron oxide nanoparticles was proposed. Iron oxide nanoparticles were synthesized through the co-precipitation method followed by functionalization with tetraethyl orthosilicate (TEOS) and 3-aminopropyl silane (APTES) to obtain Fe₃O₄@SiO₂@APTES. This composite was characterized through different techniques, including vibrating sample magnetometer, dynamic light scattering, zeta potential, FTIR, SEM, XRD, and BET. Variables studied were pH, temperature, sorbent amount, sonication time, and sample and eluent volume affecting the sorption efficacy of freshly synthesized sorbent. Plackett–Burman design was utilized for the identification of significant factors for microextraction of target analyte, while the central composite design was utilized for the optimization of significant factors. Detection and quantification limits obtained were 0.17 and 0.58 μgL⁻¹, respectively, with an enhancement factor of 83.5. Under optimum conditions, Fe₃O₄@SiO₂@APTES showed good stability even after >80 adsorption/desorption cycles run while maintaining over 96% analyte recoveries. The developed method was validated by assessing certified reference materials and standard addition methodology for Cd²⁺ detection in real samples. To confirm the precision, repeatability (RSD_r) and reproducibility (RSD_R) were calculated and found as <3.0 (n = 7) and <7.5 (n = 15), respectively. Furthermore, in accordance with the ISO/IEC 17025 recommendations, the validation was also confirmed through a “bottom-up” approach while considering all possible uncertainties in data.