A rapid, simple, and dependable method was developed and validated for the simultaneous determination of atrazine, pendimethalin, and trifluralin in fish samples. Target analytes were extracted and purified by the modified QuEChERS method prior to analysis. Ultrasound-assisted extraction (10 min) was used to improve the extraction efficiency of classical acetonitrile extraction. The organic phase was then cleaned using dispersive solid-phase extraction with 150 mg primary secondary amine and 100 mg C18-bonded silica sorbents. GC with electron capture detection was used for determination. The method resulted in good linearity (R2 = 0.9973–0.9998) and low limits of detection and quantification (0.015–0.60 and 0.050–2.0 μg kg−1). Recoveries ranged from 76.8 to 94.6% with repeatability between 2.3 and 3.8% and reproducibility between 3.4 and 4.8%. The performance parameters demonstrated the method adequacy for the detection and quantification of atrazine, pendimethalin, and trifluralin residues in freshwater fish.
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