The application of magnetized graphene (G) layers synthesized on the carbon nanofibers (CNFs) (m-G/CNF) was investigated as novel adsorbent for the magnetic solid-phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs) in water samples followed by gas chromatography-flame ionization detector (GC-FID). Six important parameters, affecting the extraction efficiency of PAHs, including: amount of adsorbent, adsorption and desorption times, type and volume of the eluent solvent and salt content of the sample were evaluated. The optimum extraction conditions were obtained as: 5min for extraction time, 20mg for sorbent amount, dichloromethane as desorption solvent, 1mL for desorption solvent volume, 5min for desorption time and 15% (w/v) for NaCl concentration. Good performance data were obtained at the optimized conditions. The calibration curves were linear over the concentration ranges from 0.012 to 100ngmL(-1) with correlation coefficients (r) between 0.9950 and 0.9967 for all the analytes. The limits of detection (LODs, S/N=3) of the proposed method for the studied PAHs were 0.004-0.03ngmL(-1). The relative standard deviations (RSDs) for five replicates at two concentration levels (0.1 and 50ngmL(-1)) of PAHs were ranged from 3.4 to 5.7%. Appropriate relative recovery values, in the range of 95.5-99.9%, were also obtained for the real water sample analysis.
The stainless steel mesh, in the form of the disk, was coated with graphene oxide and poly(dimethylsiloxane) (GO-PDMS) by sol-gel technique. The coated stainless steel meshes are loaded in the mini-column as solid-phase extraction cartridge for the fast isolation and preconcentration of polycyclic aromatic hydrocarbons (PAHs) from real water samples. The extracted PAHs (naphthalene, acenaphthene, acenaphthylene, anthracene, benz[a]anthracene, fluorene, and pyrene) were quantified by gas chromatography-mass spectrometry. The operation parameters affecting the extraction efficiency including sample volume, desorption conditions, and ionic strength were investigated. At optimized conditions, the linearity of this method is obtained from 0.001 to 20 ng mL-1 with 0.2 to 1.0 pg mL-1 limit of detection. For 5 replicates at 3 spiking levels (0.1, 1, and 10 ng mL-1), the relative standard deviations between 4.0 and 6.3% were achieved. The absolute extraction recovery varied from 89.1 to 94.7%. The enrichment factors were in the range of 2227-2367. The method has been employed in the determination of PAHs in the real water samples including well water, tap water, river water, and wastewater. Relative recoveries are between 95.2 and 100.9%. Graphical abstractSchematic representation of the SPE procedure using the self-assembly SPE cartridge.