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<b>Background:</b> Cadmium (Cd) is a very toxic and carcinogenic heavy metal even at low levels and it is naturally present in water as well as in food. <b>Methods:</b> A new polyvinyl benzyl xanthate (PvbXa) was synthesized and used as a new adsorbent in this work. It contains pendant sulfide groups on the main polystyryl chain. Using this new adsorbent, PvbXa, a vortex-assisted dispersive solid-phase microextraction (VA-dSPµE) procedure was developed for the determination of cadmium from food and water samples via flame atomic absorption spectrophotometry (FAAS). Synthesized PvbXa was characterized by ¹H Nuclear magnetic resonance (NMR) Spectroscopy, Fourier Transform Infrared Spectroscopy (FTIR), and X-ray Photoelectron Spectroscopy (XPS). The different parameters of pH, sample volume, mixing type and time, sorbent amount, and eluent time were optimized using standard analytical methods. <b>Results:</b> The optimized method for assessment of Cd in food and water samples shows good reliability. The optimum conditions were found to be a 0.20–150 µg L⁻¹ linear range, 0.06 µg L⁻¹ LOD, 0.20 µg L⁻¹ LOQ, 4.3 RSD %, and a preconcentration factor of 160. <b>Conclusions:</b> The statistically experimental variables were utilized using a central composite design (CCD). The present method is a low-cost, simple, sensitive, and very effective tool for the recovery of Cd.