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Electrosorption-enhanced solid-phase microextraction (EE-SPME) based on activated carbon fiber (ACF) was developed for determination of aniline in aqueous solution. A porous ACF, served as working electrode in electrosorption procedure, was prepared and attached to a commercial manual SPME device. Parameters affecting the adsorption efficiency were investigated. Under optimized condition, which was 400mV electrosorption potential, 0.01M Na₂SO₄ electrolyte, pH 7, and electrosorption at 40°C for 10min, the method exhibited wide linear range (0.1–100μgL⁻¹, R²=0.9980), good repeatability of adsorption (RSD 6.15%, n=6), and low detection limit (0.02μgL⁻¹). The feasibility of the method was evaluated by analyzing lake water spiked with aniline. Comparison was made with direct immersion (DI) ACF-SPME without electrosorption enhancement. The proposed procedure was demonstrated to be a …