In the present study, we have developed a novel dispersive liquid–liquid microextraction (DLLME) based on microwave-assisted DLLME (MADLLME) usingionic liquidsfor the separation of environmentally-relevant pyrethroidpesticidesfrom various aqueous milieux.High-performance liquid chromatography(HPLC) was employed for the detection and quantitative tracking of thepesticides. Six different ILs were preliminarily tested asextractionsolventsagainst four representative model pyrethroids. The optimization of the current method was derived by consideration of the dispersalsolvent,ionic liquidchoice,extractioncontainer material, aqueous-phase pH, and microwave conditions (particularly, the applied power and irradiation time). Optimal results were achieved usingmethanolas a dispersalsolventwith trioctylmethylammonium bis(trifluoromethylsulfonyl)imide ([N₈₈₈₁][Tf₂N]) as the extractionsolventat a microwave power of 200 W for 60 s. A number of spikedfoodsamples (e.g., honey, milk, assorted fruits) were also tested using MADLLME, with excellent recoveries achieved from these complex matrices as compared to DLLME alone.