Magnetic extraction offers a rapid and low-cost solution to microplastic (MP) separation, in which we magnetize the hydrophobic surface of MPs to separate them from complex environmental matrices using magnets. We synthesized a hydrophobic Fe-silane based nanocomposite (Fe@SiO2/MDOS) to separate MPs from freshwater. Pristine and weathered, polyethylene (PE) and tire wear particles (TWP) of different sizes were used in the study. The weathering of MPs was performed in an accelerated weathering chamber according to ISO 4892-2:2013 standards that mimic natural weathering conditions. The chemical properties and morphology of the Fe@SiO2/MDOS, PE and TWP were confirmed by Fourier transform infrared spectroscopy and Scanning electron microscopy, respectively. The thermal properties of PE and TWP were evaluated by Thermogravimetric analysis. Using 1.00 mg of Fe@SiO2/MDOS nanocomposite, 2.00 mg of pristine and weathered PE were extracted from freshwater; whereas, using the same amount of the nanocomposite, 7.92 mg of pristine TWP and 6.87 mg of weathered TWP were extracted. The retrieval of weathered TWP was 13% less than that of pristine TWP, which can be attributed to the increasing hydrophilicity of weathered TWP. The results reveal that the effectiveness of the magnetic separation technique varies among different polymer types and their sizes; the weathering of MPs also influences the magnetic separation efficiency.