A nanocomposite comprised of Fe3O4 magnetic nanoparticles（MNPs） and multi-walled carbon nanotubes（MWCNTs） was synthesized,and used as adsorbent in the determination of 16 PAEs in water samples by magnetic solid phase extraction（MSPE）and quantification by gas chromatography-mass spectrometry（GC-MS）.The synthesis nano material was characterized by Fourier transform infrared spectroscopy.The factors affecting the extraction efficiency,such as type and amount of elution solvent,desorption time,adsorption time and pH value of water sample,were investigated.The optimized conditions were as follows:elution solvent:1 mL toluene-acetone（1∶4）;desorption time:1 min;adsorption time:3 min;pH of water sample:5.0-7.0.The detection limits（S/N=3）for 16 PAEs were in the range of 0.035-0.255 μg/L and the quantitation limits（S/N=10） were 0.115-0.845 μg/L.The developed method was successfully applied in the analysis of 16 PAEs in tap water,lake water and river water.The recoveries at 3 spiked levels ranged from 87% to 112% with RSDs of 1.3%-11.9%.The results demonstrated that the MSPE method could be rapidly and effectively used in the monitoring of trace PAEs contaminants in water sample.