Synthesis of GO/γ-Fe₂O₃ for Application in Solid-Phase Dispersive Magnetic Microextraction for Determination of Pesticides at Ultra-Trace Levels in River Water Samples by HPLC-DAD

Nanocomposites of GO/γ-Fe₂O₃ were used for magnetic dispersive solid-phase microextraction (m-d-μ-SPE) of six pesticides from river water samples, followed by the determination using high performance liquid chromatography-diode array detection. The synthesis of the nanocomposites is described and characterized using Fourier transform-infrared spectroscopy, X-ray diffraction, and scanning electron microscopy. A central composite design was used to optimize the extraction time, sample solution pH, and adsorbent amount. The solvent type and volume for desorption and the effect of the ionic strength for adsorption were also investigated. The optimum adsorption conditions were achieved at 84 min of extraction time, pH 5.4, 115 mg of absorbent, and 1% (m/v) of NaCl, while the desorption solvent selected was 1.0 mL of methanol-acetic acid (9:1, v/v). The limits of detection ranged from 0.1 to 0.9 μg L^-1, and a good precision was achieved with relative standard deviation (RSD) lower than 7.6% (n = 10). The accuracy of the method was accessed by recovery tests ranging from 82 to 117% (n = 3, RSD < 8%).

Keywords:
graphene oxide; pesticides; pre-concentration; high-performance liquid chromatography; experimental design