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.

Highlights

  • Vegetables and fruits are a significant source of vitamins and minerals

  • Liquid-phase microextraction (LPME) is an alternative miniaturized sample preparation technique that overcomes many disadvantages of liquid-liquid extraction (LLE). e recently developed methodology (LPME) has many advantages, such as it significantly reduced the volume of hazardous organic solvents, is environmentally benign, is inexpensive, and is fast for extraction/preconcentration of multiresidue pesticides from complex matrices compared with the conventional method [9,10,11]

  • Microextraction techniques such as reversedphase ultrasonic assisted liquid-liquid microextraction (RPUALLME) [11], liquid-phase microextraction and the freezing of deep eutectic solvent (LPME-FDES) [12], vortexassisted dispersive liquid-liquid microextraction based on the freezing of deep eutectic solvent (VADLLME−FDES) [13], and sonication and dispersive liquid-liquid microextraction based on the solidification of floating organic drop (SDLLME-SFO) [14] have been developed for the determination of organic and inorganic compounds in different matrices

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Summary

Introduction

Vegetables and fruits are a significant source of vitamins and minerals. fruits and vegetables can be sources of pollutants such as pesticides, which may be found on the peel or penetrate and translocate into plants via the xylem or phloem [1]. E recently developed methodology (LPME) has many advantages, such as it significantly reduced the volume of hazardous organic solvents, is environmentally benign, is inexpensive, and is fast for extraction/preconcentration of multiresidue pesticides from complex matrices compared with the conventional method [9,10,11]. Microextraction techniques such as reversedphase ultrasonic assisted liquid-liquid microextraction (RPUALLME) [11], liquid-phase microextraction and the freezing of deep eutectic solvent (LPME-FDES) [12], vortexassisted dispersive liquid-liquid microextraction based on the freezing of deep eutectic solvent (VADLLME−FDES) [13], and sonication and dispersive liquid-liquid microextraction based on the solidification of floating organic drop (SDLLME-SFO) [14] have been developed for the determination of organic and inorganic compounds in different matrices. To assess the proposed method’s applicability, it was applied for the quantitative determination of target pesticides in apples, tomato, pear, and melon

Materials and Methods
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