Enhanced extraction of organophosphorus pesticides from fruit juices using magnetic effervescent tablets composed of the NiFe2O4@SiO2@PANI-IL nanocomposites

Abstract

The reported ionic liquid (IL)-based magnetic effervescent tablets are a result of direct addition of ILs and magnetic nanoparticles (MNPs). In effervescent reaction-enhanced microextraction procedures, the dissociation between ILs and MNPs easily leads to loss of ILs due to aqueous solubility, thereby decreasing the extraction efficiency. Herein, we attached a hydrophilic IL ([BMIM]Br) onto the surface of NiFe₂O₄@SiO₂@polyaniline (NiFe₂O₄@SiO₂@PANI-IL) to prepare novel core–shell-like multi-layer nanocomposites. Magnetic effervescent tablets were composed of Na₂CO₃ as an alkaline source, tartaric acid as an acidic source and as-synthesized nanocomposites as an extractant. The nanocomposites were used in an effervescent reaction-enhanced magnetic solid-phase extraction (ERMSE) for the extraction of four organophosphorus pesticides (OPPs) in fruit juices prior to HPLC-DAD detection. Under optimized conditions, this method provided low limits of detection (0.06–0.17 μg L⁻¹), high recoveries (80.6–97.3%) and excellent precision (1.1–5.2%) for OPP quantification in five fruit juices. Notably, the three-layer core–shell nanocomposites were efficiently recycled for at least eight extraction cycles with a recovery loss of <10%. The novelty of this study lies in: (1) for the first time, the ILs-based hybrid magnetic nanocomposites were prepared with appropriate pore size/volume and more active sites for OPPs; (2) the combination of the nanocomposites with effervescent tablets realizes rapid dispersion of CO₂ bubbles, and convenient magnetic separation/collection into one synchronous step; and (3) due to there being no requirement of electrical power, it is feasible for use in field conditions. Thus, the ERMSE method has excellent potential for conventional monitoring of trace-level OPPs in complex fruit juice matrices.