In this study, an efficient preconcentration method was presented that is based on dispersive liquid‐liquid microextraction taking the advantage of newly synthesized phosphonium deep eutectic solvents used as extractants and ultrasound probe as a dispersing agent. The extracts obtained were analyzed by high‐performance liquid chromatography. To optimize the five most important factors for the microextraction procedure a central composite design plan was used. Under optimal conditions (140 μl of extractant, 60 mg of NaCl, pH = 2.0, 120 s of extraction time with ultrasound probe as the dispersing agent, 16 min of centrifugation for phase separation), the proposed method allowed to achieve good precision with RSD between 3.2% and 9.7% at 1.0, 5.0 and 40.0 ng ml levels. The preconcentration factors were equal to 42, 39, and 41, and the limits of detection 0.128, 0.103, and 0.135 ng/ml for dicamba, 2‐methyl‐4‐chlorophenoxyacetic acid, and 2‐methyl‐4‐chlorophenoxypropionic acid, respectively. The proposed method was successfully applied for the determination of chlorophenoxy acid herbicides in water samples from drainage ditches with a good recovery in the range of 70%–93%.
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