Microplastics and chlorpyrifos are widespread pollutants that threaten aquatic ecosystems and human health, necessitating effective detection, quantification, and removal strategies. Microplastics accumulate in marine organisms, entering the food chain, while chlorpyrifos, a neurotoxic pesticide, poses severe risks, particularly to children's neurodevelopment. This study utilizes a magnetic adsorption approach for their simultaneous removal. Iron oxide nanoparticles (Fe₃O₄) were synthesized via co-precipitation, coated with carbon (C@FeO), and integrated into two-dimensional metal-organic frameworks (2D MOFs) to form a nanopillared heterostructure (2D MOF@C@FeO). Batch adsorption experiments assessed the removal efficiency under varying material dosages, contact times, and pollutant concentrations, achieving rapid and high adsorption within 60 minutes. Microplastics and chlorpyrifos were identified and quantified using Differential Light Scattering (DLS), UV-Vis spectroscopy, Master Sizer, and Gas Chromatography-Mass Spectrometry (GC-MS). The findings highlight the potential of 2D MOF@C@FeO as an effective adsorbent for dual pollutant removal, contributing to water safety and sustainability. By mitigating waterborne contaminants, this study supports public health, reduces treatment costs, and enhances water quality for industrial and domestic use.