There is a growing interest in utilization of abundantly available materials, bio-mass or industrial byproducts, as precursors for the preparation of carbon materials. Short hemp fibers, acquired as waste from textile production, were used as low-cost precursor for production of carbon materials as a sorbent in the solid-phase extraction, for pesticide analysis in water samples. Different carbon materials were prepared by carbonization of unmodified and chemically modified hemp fibers. Activation of carbonized materials with potassium hydroxide improves sorption properties of carbonized hemp fibers by increasing the specific surface area (up to 2192 m(2)/g) and the amount of surface oxygen groups. The following parameters that may affect the solid-phase extraction procedure efficiency were optimized: different elution solvents and the pH value of pesticide solution. Extracts were analyzed by liquid chromatography-tandem mass spectrometry technique. For this study pesticides belonging to the different chemical classes were chosen. Obtained results indicate that carbonized and activated hemp fibers could be successfully applied as a solid-phase sorbent for the pesticide analysis in water samples. (C) 2012 Elsevier B.V. All rights reserved.