<p>A magnetic dispersive solid-phase extraction (M-d-SPE) technique was developed using a magnetic nanocomposite graphene oxide (Fe₃O₄@GO) for preconcentration of carbamates and organophosphate residues. The detection was performed via ultraperformance liquid chromatography equipped with a photodiode-array detector. The synthesis nanocomposite adsorbent was achieved through co-precipitation method under alkaline condition. The evaluation of the nanocomposite adsorbent was conducted, confirming the successful synthesis of the prepared adsorbent and its structural integrity. The parameters influencing extraction efficiency were optimized. The optimum synthesized and extraction conditions were 1:3 GO base ratio, Fe₃O₄@GO adsorbent 100&#xa0;mg, acetonitrile (250 µL) as the desorption solvent, a sample volume of 60&#xa0;mL at pH 5, NaCl 20%w/v. The method exhibited good linearity (5–1000 µg L⁻¹) with the coefficient of determination (<i>R</i>²) greater than 0.99, low detection limits (0.7 to 1.0 µg L⁻¹), low limits of quantification (2.3 to 3.3 µg L⁻¹), and high precision (relative standard deviation (RSD) less than 4.04%). Recoveries in food and environment samples ranged from 60.45 to 119.95%. The greenness and blueness assessment tools were applied to confirm that M-d-SPE qualifies as a robust green chemistry method. The proposed method presents several benefits, including low cost, characterized by cost-effectiveness and low solvent usage. This approach serves as a sustainable alternative to traditional methods for evaluating pesticide residues.</p>