Multiclass Pesticide Residue Analysis in Fruit and Vegetable Samples by Combining Acetone-Based Salting-Out Assisted Extraction with Dispersive Liquid-Liquid Microextraction

Abstract

Isolation and enrichment of multiclass pesticides’ residue, namely, fungicides (benalaxyl), herbicides (atrazine), carbamate insecticides (carbofuran), organophosphate insecticides (chlorpyrifos), organochlorine insecticides (4,4′-DDT), and pyrethroid insecticides (bifenthrin), were made by combining acetone-based salting-out assisted extraction with the dispersive liquid-liquid microextraction (SADLLME) method, followed by high-performance liquid chromatography-diode array detection (HPLC-DAD). The effect of the type and volume of the extraction solvent in the pretreatment step, the volume of the disperser solvent (acetone extract), the type and volume of the extraction solvent, pH, and salt addition in the DLLME procedure was studied. Good coefficient of determination (R2 ≥ 0.9964) was obtained for all the target analytes. The limits of detection and quantification limits were between 2.1 and 4.5 and 5.7 and 12.9 µg/kg, respectively, with adequate enrichment factors ranging from 37.6 to 191. The recoveries of spiked blank tomato ranged from 86.8 to 109.5%. The limit of quantification of the proposed method was lower than the maximum residue limits set by the European Union. The repeatability and reproducibility of precisions ranged between 2.9 and 8.0 and 4.9 and 9.5%, respectively. The optimized and validated method was applied to quantify pesticides in tomato, pear, apple, and melon obtained from different markets. However, all target compounds studied in this work were not detected in any real samples applied. Overall, the work results revealed that the proposed method is useful for the sample extraction and preconcentration of the target analytes from fruits and vegetables.