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In this study, a novel method using a phosphonium‐based deep eutectic solvent coupled with vortex‐assisted liquid–liquid microextraction was investigated for the enrichment and separation of five benzoylurea insecticides in olive oil. The experimental factors affecting the extraction efficiency, including the extractant type, deep eutectic solvent volume, extraction time, and extraction mode, were optimized. Under optimal conditions, good linearity was observed for all target analytes, with correlation coefficients (r) ranging from 0.9971 to 0.9998; the limits of detection were in the range of 1.5 to 7.5 μg/L, and the recoveries of analytes using the proposed method ranged between 66.9 and 111.0%. The simple, rapid, and effective method was successfully applied for detecting target analytes in olive oil sample.

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