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A novel SPME fiber was prepared by electrophoretic deposition of titanium dioxide nanoparticles (nano-TiO₂) on a stainless steel wire. It was used in the direct immersion solid-phase microextraction (DI-SPME) of four phthalate esters from aqueous samples prior to gas chromatographic (GC) analysis. The effects of various parameters on the efficiency of the SPME process such as the mode of extraction, extraction temperature, film thickness of the SPME fiber, salt content, extraction time and stirring rate were investigated. The comparison of the fiber with another homemade poly(3,4-ethylenedioxythiophene)-TiO₂ (PEDOT-TiO₂) nanocomposite fiber and a commercial polydimethylsiloxane (PDMS) fiber showed the better extraction efficiency of the nano-TiO₂ fiber for phthalate esters. Under optimized conditions, the limit of detection (LOD) for the phthalate esters varied between 0.05 and 0.12μgL⁻¹. The inter-day …