Magnetic Fe3O4 graphene oxide nanocomposite was synthesized by chemical coprecipitation method and characterized by scanning electron microscopy, Fourier transform infrared spectra and X-ray diffraction. A simple, rapid, convenient and environmentally friendly method was developed for separation and pre-concentration of trace amounts of bisphenol A, naproxen and triclosan in wastewater samples by high performance liquid chromatography with magnetic Fe3O4 graphene oxide nanocomposite as the adsorbent for magnetic solid-phase extraction. Various parameters possibly influencing the extraction performance such as amount of the adsorbent, extraction time, sample pH and elution conditions were optimized. Under the optimal working conditions, the developed method showed good linearity (R > 0.9997) in the range of 1–200 μg/L, and the limits of detection are between 0.5 and 0.8 μg/L. The enrichment factors are in the range of 81–89. The repeatability of the method, expressed as relative standard deviation, is 3.36–4.26%.