In this work, iron (III) oxinate magnetic nanocomposite was synthesized and employed as an efficient sorbent for the magnetic dispersive solid‐phase extraction of some polycyclic aromatic hydrocarbons from honey samples. In the following, dispersive liquid–liquid microextraction procedure was used for further preconcentration of the analytes. The prepared sorbent was characterized using Fourier transform infrared spectrophotometry, X‐ray diffractometry, vibrating sample magnetometry, energy dispersive X‐ray spectroscopy, and scanning electron microscopy. The results verified the successful formation of the magnetic sorbent. In the extraction process, the sorbent was added into an aqueous solution and the mixture was vortexed. After completing the adsorption process, the supernatant phase was separated in the presence of a magnet and the analytes adsorbed onto sorbent were eluted by acetonitrile. Then, microliter‐level 1,1,1–trichloroethane was mixed with the obtained acetonitrile and injected into NaCl solution. Finally, one microliter of the sedimented phase was injected into gas chromatography‐flame ionization detector after centrifugation. Under the optimum conditions, a great repeatability (relative standard deviation equal or less than 5 and 6% for intra– and interday precisions, respectively), acceptable extraction recoveries (59–84%), high enrichment factors (118–168), and low limits of detection and quantification (0.16–0.36 and 0.56–1.22 ng/g, respectively) were acquired.
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