Magnetic solid-phase extraction using Seniff base ligand supported on magnetic nanoparticles as sorbent combined with dispersive liquid-liquid microextraction for the extraction of phenols from water samples

摘要

In this work, the magnetic sorbent was developed by covalent binding of a Schiff base ligand, N,N'-bis(3-salicyliden aminopropyl)amine (salpr), on the surface of silica coated magnetic nanoparticles (Salpr@SCMNPs). The core-shell nanoparticle was applied for the magnetic solid-phase extraction (MSPE) combined with dispersive liquid-liquid microextraction (DLLME) of phenolic compounds from water samples prior to gas chromatography-flame ionisation detector (GCFID). Characterisation of the Salpr@SCMNPs was performed with different physicochemical methods such as Fourier transform infrared (FT-IR), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). Variables affecting the performance of both extraction steps such as pH of the water sample, the sorbent amount, the desorption conditions, the extraction time; and extraction solvent were studied. Under the optimised conditions, the analytical performances were determined with a linear range of 0.01-100 ngmL(1) and a limit of detection at 0.003-0.02 ngmL(1) for all of the analytes studied. The intra-day (n=5) and inter-day (n=3) relative standard deviations (RSD%) of three replicates were each demonstrated in the range of 6.9-8.9% and 7.3-10.1%, respectively. The proposed method was executed for the analysis of real water samples, whereby recoveries in the range of 92.9-99.0% and RSD% lower than 6.1% were attained.