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Co-exposure to n-hexane and methyl ethyl ketone (MEK) may induce neurotoxicity in humans. Since biomonitoring of exposed chemicals is a powerful hygienic way of controlling chemical risk, a new molecularly imprinted polymer (MIP) is reported in this study. Polymerization was carried out upon the surface of magnetic silica aerogel (Si@Fe₃O₄) using 2-octanone as a dummy template to prepare Si@Fe₃O₄-MIP. The synthesized MIP was characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectrometry thermogravimetric analysis (TGA), Brunauer–Emmett–Teller (BET) analysis, and vibration sample magnetometry (VSM). The reported method was utilized for the selective extraction of n-hexane and MEK from humane urine using gas chromatography – flame ionization detection (GC-FID). The highest selectivity coefficient of Si@Fe₃O₄-MIP was obtained for n-hexane and MEK …