A new Fe3O4/polyaniline nanoparticle (PANI) material has been successfully developed as magnetic solidphase
extraction sorbent in dispersion mode for the determination of methylmercury (MeHg) in aqueous
samples, via quantification by gas chromatography/mass spectrometry (GC–MS). The resultant core–shell
magnetic solid-phase extraction nanoparticle (MSPE-NP) sorbent was characterized by scanning electron
microscopy (SEM), energy dispersive X-ray spectrometry (EDS) and Fourier transform-infrared (FTIR)
spectroscopy. Fe3O4/PANI composites showed fibrous structure with diameters between 50 and 100 nm
for fibers. The MSPE-NP process involved the dispersion of the Fe3O4/PANI nanoparticles in water samples
with sonication, followed by magnetic aided retrieval of the sorbent and then, solvent (hexane) desorption
of extracted MeHg for GC–MS analysis. The extraction, derivatization and adsorption conditions
were optimized by selecting the appropriate extraction parameters including the amount of sorbent,
extraction time, derivatizing reagent volume and extraction solvent. The calibration graph was linear in
the concentration range of 0.5–300 ng mL−1 (R2 > 0.993) with detection limit of 0.1 ng mL−1 (n = 3), while
the repeatability was 4.1% (n = 5). Enrichment factor was obtained as 91. Seawater sample was analyzed
as real sample and good recoveries (>98%) were obtained at different spiked values.