A solvent-free mechanochemical extraction (SFMCE) technology was applied to the extraction of chondroitin sulfate (CS) from shark cartilage. This process was carried out via mechanical pretreatment (MPT) and mechanochemical treatment (MCt) in AGO-2 high-intensity planetary activator at room temperature under solvent-free condition. The yield of CS was increased from 8.50 +/- 0.16% to 9.33 +/- 0.14% and the purity of product was improved from 86.4 +/- 0.88% to 95.1 +/-0.65%. The effectiveness of the MCT was confirmed by HPLC-ELSD analysis. The energy cost was decreased obviously due to the decrease of extraction time from 3 h to 3 min. SFMCE method was proved to be a high-efficient and energy-saving technique. (C) 2009 Elsevier B.V. All rights reserved.