Ultrasound-assisted magnetic nanofluid-based liquid-phase microextraction was coupled to GC-MS in a method for simultaneous determination of the pyrethroid insecticides permethrin, deltamethrin, and cypermethrin. A highly efficient extraction solvent called "magnetic nanofluid (MNF)" is introduced for preconcentration of pyrethroids. The MNF consists of magnetic multiwalled carbon nanotubes (MMWCNTs) and deep eutectic solvent. Following microextraction, the MNF was detached by an external magnet from the medium without the need for centrifugation. 2-Pyridinecarboxamide, choline chloride, and anhydrous ferric chloride were used for the synthesis of the deep eutectic solvent. The effects of pH value, volume of MNF, sonication time, sample volume, and ionic strength, type and amount of back extraction solvent were investigated. Under optimum conditions of MNF volume of 50 μL, time of 5 min, 100 μL acetone as back extraction solvent, NaCl concentration of 1 mol.L and sample volume of 30 mL, the detection limits are 2.8, 2.7 and 2.0 ng·mL for permethrin, deltamethrin and cypermethrin, respectively. The linear response ranges are between 0.01 and 250 ng·mL, and relative standard deviations (for n = 7) are 3.5, 3.2 and 2.8%. The method was successfully applied to the determination of trace levels of permethrin, deltamethrin and cypermethrin in (spiked) milk samples. Graphical abstract Schematic representation of ultrasound assisted magnetic nanofluid-based liquid phase microextraction separation/preconcentration of permethrin, deltametrin, and cypermethrin residues in milk using GC-MS.