Nitrogen-doped activated carbon fibers (ACFs) were prepared by chemical vapor deposition using melamine powder and acetonitrile for introducing quaternary nitrogen on the commercial ACFs, subsequently heated at 950 °C and activated by steam. Adsorption experiments of nitrate in aqueous solution were also conducted to evaluate adsorption capacity of the prepared ACFs using ion chromatography. The amount of introduced nitrogen content and nitrogen species on activated carbon fibers was examined by CHN elemental analyzer and X-ray photoelectron spectroscopy, respectively. As a result, adsorption capacity of quaternary nitrogen-doped ACF (ST-ML-AN-ST) was 0.75mmol/g, indicating ca. two-times higher than that of untreated ACF (0.38mmol/g). According to the adsorption data, the Langmuir isotherm model was the best fit. The prepared samples were also regenerated using hydrochloric acid. After regeneration, the adsorption capacity of the nitrogen-doped ACF (ST-ML-AN-ST) showed ca. 80% on average, implying that a portion of nitrates was adsorbed on the prepared ACFs irreversibly.