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A novel electrospun composite nanofiber-based adsorbent (polyurethane/polystyrene-silica) was fabricated, characterized, and used in the headspace solid-phase microextraction of the acetylated derivatives of chlorophenols in water samples before gas chromatography with micro electron capture detection. The surface morphology, chemical composition, thermal stability, and structure of the fibers were investigated by scanning electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, and Brunauer-Emmett-Teller and Barrett-Joyner-Halenda techniques. The effect of the main parameters influencing the efficiency of the method including extraction temperature, salt concentration, and extraction time was investigated and the optimized conditions were obtained. The linear dynamic ranges were 0.1-800 ng/mL. The relative standard deviations (n = 3) and the limits of detection were 2.64-9.57% and 0.0234-0.830 ng/mL, respectively. The relative recoveries for real samples (river water and sewage of our university campus) were between 90.8 and 111%.

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