Magnetic solid-phase extraction based on GO/Fe₃O₄ coupled with UPLC-MS/MS for determining nitroimidazoles and their...

A magnetic graphene oxide (GO/Fe₃O₄) nanocomposite was synthesized in one step by a chemical coprecipitation method, which was further used for magnetic solid-phase extraction (MSPE). This study aimed to combine GO/Fe₃O₄ with ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to detect the nitroimidazoles (NDZs) and their three major metabolites in honey samples. GO/Fe₃O₄ was characterized by transmission electron microscopy (TEM), Fourier transform-infrared (FT-IR) spectroscopy, and magnetic property measurement system (MPMS), and the influencing parameters such as adsorbent amount, pH of the dissolved sample solution, sample volume, type and volume of the eluent, shaking speed, and adsorption and desorption time were optimized. Under the optimized conditions, the limits of detection (LOD) and quantitation (LOQ) of the method were 0.003-0.08 μg kg^-1 and 0.009-0.3 μg kg^-1, respectively, with good linearity reported in the range of 0.5-20 μg kg^-1 (R² ≥ 0.9991). The average recoveries of 10 analytes were in the range of 66.0%-90.8% with relative standard deviations (RSD) lower than 6.9% (n = 6). The preparation of GO/Fe₃O₄ and the extraction process were convenient and rapid, and consumed small amounts of organic solvents. The optimized method was successfully applied for extracting NDZs and their three major metabolites from honey samples with good accuracy.