A simple, rapid, and efficient pretreatment method of mefentrifluconazole enantiomers in cereal samples was established by dispersive liquid–liquid microextraction coupled with ultra-high-performance liquid chromatography-diode array detector (UHPLC-DAD). In this study, a novel ternary magnetic deep eutectic solvent (MDES) [octyltrimethylammonium bromide][cobalt chloride][acetic acid] was synthesized as the extractant. Acetic acid was used as the dispersant to promote the in situ dispersion of binary MDES [octyltrimethylammonium bromide][cobalt chloride]. The microdroplets of binary MDES containing mefentrifluconazole were separated by an external magnet. Device-assisted dispersion and time-consuming centrifugation steps were eliminated to ensure simplicity and rapidity of the pretreatment. Good linearity ranging from 0.01 μg g−1 to 2 μg g−1 was obtained. The extraction recovery varied from 82.9 to 95.0%. The limit of detection was 0.003 μg g−1. Finally, this established approach has been applied for the enantioselective detection of chiral mefentrifluconazole in corn, rice, wheat, millet, and sorghum samples.
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