Abstract

Neonicotinoid insecticides have raised a lot of societal concerns due to their environmental ubiquity and unique mode of action. Therefore, it is of great research interest to monitor their occurrence in the environmental waters. However, these compounds exist at low concentrations that is below instrument detection limits. This study reports the applicability of magnetic poly (3 aminobenzoic acid)-based activated carbon (Fe3O4@PABA/AC) composite as an adsorbent in dispersive magnetic solid-phase microextraction (d-MSPME) of neonicotinoid insecticides from wastewater and river water samples. The as-synthesized adsorbent was characterized and confirmed by Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, Brunauer–Emmett–Teller and X-ray diffraction spectroscopy. The analytes of interest were detected and quantified by high-performance liquid chromatography coupled with diode array detector (HPLC–DAD). The parameters affecting the extraction and preconcentration processes, such as pH, extraction time, mass of adsorbent, desorption time and eluent volume, were optimized using fractional factorial design and central composite design. Under optimum conditions, the limits of detection and quantification were in the ranges of 0.41–0.82 µg L−1 and 1.4–2.7 µg L−1, respectively. The linearity ranged from 1.4–700 µg L−1 with correlation of determination (R2) values varied between 0.9933 and 0.9987. The intra-day and inter-day precisions were 0.35–0.75% and 1.7–5.5%, respectively. The spike recovery experiments were conducted to evaluate the accuracy of the d-MSPME analytical method in real samples, and the percentage recoveries ranged from 86.7 to 99.2%. Therefore, this method shows great potential applicability in preconcentrating the pollutants from the environment.

Highlights

  • Access to clean water has become a global concern

  • The FTIR spectrum of PABA shows the absorption bands at 3408 ­cm−1 was assigned to the overlapping stretching vibrations of carboxylic O–H and secondary amine N–H, while the bands at 1750, 1589, and 1483 ­cm−1 were ascribed to the stretching vibrations of C=O, ­COO− asymmetric stretch and −COO− symmetric stretch of the carboxylic group, Fig. 1 Schematic diagram summarizing the experimental procedures

  • The dispersive magnetic solid-phase microextraction (d-MSPME) showed a great potential as a preconcentration method for the selected neonicotinoid insecticides. ­Fe3O4@PABA/AC nanocomposite was characterized using FTIR, SEM, TEM, BET and XRD

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Summary

Introduction

The remarkable increase in human population has triggered high industrialization and agricultural production to meet mankind sustainability (Munonde 2017). These activities lead to increased use of various chemical substances that are released into the environment. Neonicotinoid insecticides are a relatively new class of insecticides derived from nicotine, and they were introduced in the 1990s for insects control (Yáñez et al 2014; Farajzadeh et al 2016). They act agonistically at the nicotinic acetylcholine receptors (nAChRs) on the post-synaptic layer. These compounds are considered less toxic to mammals (Farajzadeh et al 2016; Zou et al 2019; Mahai et al 2019)

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