AbstractNine soluble polysaccharide fractions were sequentially extracted with hot water at 80, 100, and 120 °C for 3 h, and 60% aqueous ethanol containing 0.25, 0.50, 1.00, 2.00, 3.00, and 5.00% NaOH at 80 °C for 3 h from dewaxed bamboo (Dendrocalamus brandisii) sample, and their chemical compositions and physicochemical properties were examined. The sequential treatments yielded 20.6% soluble polysaccharides of the dry dewaxed bamboo material. Molecular weight and neutral sugars analysis revealed that the soluble polysaccharides were mainly composed of arabinoglucuronoxylans and amylose starch. Spectroscopy (FT-IR, 1H, 13C, and 2D-HSQC NMR) analyses suggested that the isolated arabinoglucuronoxylans from bamboo (D. brandisii) could be defined as a linear (1→4)-β-linked-xylopyranosyl backbone to which α-L-arabinofuranose units and/or short chains of 4-O-methyl-glucuronic acid were attached as side residues via α-(1→3) and/or α-(1→2) linkages. In addition, it was found that the thermal stability of polysaccharides increased with an increment of their molar mass.