This work presents as a novelty the development of a method for the simultaneous determination of organophosphorus and pyrethroid pesticides in aqueous samples using only deep eutectic solvents (DES) followed by a gas chromatography-mass spectrometry analysis. Combining 4 hydrogen bond acceptors and 6 hydrogen bond donors, 17 DES were prepared. Menthol:thymol in a 1:1 molar ratio presented the best extraction performance and was, therefore, characterized by Fourier transform infrared spectroscopy (FTIR), hydrogen-nuclear magnetic resonance (