Polypyrrole (PPy)-functionalized Fe3O4 magnetic nanoparticles (Fe3O4–PPy) were prepared and applied as magnetic solid-phase extraction (MSPE) sorbents for the extraction of polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. To achieve the optimal extraction performance, several parameters were investigated, including the amounts of sorbent, volume of desorption solvent, extraction and desorption time, inorganic salt and organic solvent content of the sample matrix. Coupled with gas chromatography/mass spectrometry (GC/MS) analysis, a rapid, sensitive and cost-effective method for the analysis of PAHs in aqueous samples was established. The low detection limits (LODs) for the target PAHs in the proposed method were in the range of 0.38 to 5.01 ng L−1, which are much lower than those LODs reported in previous methods. Good linearity of the detection method was obtained with correlation coefficients (R) between 0.9904 and 0.9992. Satisfactory reproducibility was also achieved with relative standard deviations (RSDs) less than 13.3% by an intra- and inter-day precision evaluation. The recoveries of the 10 PAHs in several environmental water samples ranged from 72.4% to 115.7% with the RSDs being less than 9.7%.
