A new green miniaturized quick, easy, cheap, effective, rugged, and safe approach was developed and used for the extraction of multiclass 16 pesticides in milk before gas chromatography analysis. The miniaturization of method reduced the consumption of chemical reagents and samples. Magnetic three-dimensional graphene was used as sorbent in the clean-up step. Choline chloride:lactic acid (1:2) natural deep eutectic solvent was used as desorption solvent. Temperature-assisted solidification of floating menthol drop was executed for preconcentration of analytes. The method parameters including sorbent, desorption solvent, sorption and desorption times, menthol amount, pH, and ionic strength were optimized. The limit of quantification and linear range were 0.03-0.38 and 0.03-250 μg/kg, respectively. The accuracy was assessed by recovery evaluation at the spike levels of 50 and 100 μg/kg, in the range of 61-119%, with relative standard deviations within 2.1-18.2%. The method was applied to the analysis of pasteurized low and high-fat bovine milk, and various pesticide residues were detected in the concentrations range of 1.24-4.68 μg/kg. Finally, the greenness of the procedure was evaluated using the Analytical Eco-Scale. This work represents the first application of hybrid miniaturized extraction/preconcentration using a natural deep eutectic solvent and menthol to analyze pesticides.
Keywords: milk; miniaturized extraction; multiclass pesticides; natural deep eutectic solvent; solidification of organic drop.
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