In this work, the extraction of polycyclic aromatic hydrocarbons (PAHs) with an efficient poly(pyrrole-co-aniline)@graphene oxide/Fe3O4 [poly(Py-co-Ani)@GO–Fe3O4] nanocomposite followed by GC-FID is presented. In the comparison of different magnetic nanosorbents including GO–Fe3O4 and poly(Py-co-Ani)@GO–Fe3O4, the results obtained showed that the poly(Py-co-Ani)@GO–Fe3O4 nanocomposite has the highest extraction efficiency for the analytes. The sorbent was characterized by vibrating sample magnetometry (VSM), Fourier transform infrared spectroscopy (FT-IR) and transition electron microscopy (TEM). The optimal extraction conditions include: sorbent amount, 35 mg; sorption time, 10 min; salt concentration, 30% w/w; type and volume of the eluent, toluene, 1 mL; elution time, 5 min. Under the optimal extraction conditions, limits of detection (LODs) and the linear dynamic ranges were achieved in the range of 0.003–0.01 ng mL−1 and 0.01–200 ng mL−1, respectively. The absolute extraction recovery (ER%) and relative standard deviations (RSD%) were in the range of 50.4–78.3% and 5.2–8.5%, respectively. Finally, the applicability of the method was successfully confirmed by the extraction and determination of PAHs in real water samples.

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