Liquors from rice husk autohydrolyis, containing xylooligosaccharides, other saccharides, and nonsaccharide compounds, were subjected to two selected processing schemes to increase the proportion of substituted xylooligosaccharides in refined liquors. Nanofiltration through a ceramic membrane with a molecular mass cutoff of 1000 Da allowed simultaneous concentration and purification; this latter derived from the preferential removal of monosaccharides and nonsaccharide compounds. When liquors were nanofiltered to achieve a volume reduction factor of 5 operating at a transmembrane pressure of 14 bar, 58.6% of the nonsaccharide components and 20.9-46.9% of monosaccharides were kept in retentate, in comparison with 92% of xylooligosaccharides and glucooligosaccharides. When nanofiltered liquors were subjected to double ion-exchange processing, a final product with a nonsaccharide content near 9 kg/100 kg of nonvolatile components was obtained at a yield of 10.90 kg/100 kg oven dry rice husks. Alternatively, when nanofiltered liquors were subjected to ethyl acetate extraction and further double ion-exchange processing, a purified product with a nonsaccharide content of 5.66 kg/100 kg of nonvolatile components was obtained at a yield of 9.94 kg/100 kg oven dry rice husks. The nonsaccharide components remaining in the final concentrate were mainly made up of phenolic and nitrogen-containing compounds. © 2006 American Chemical Society.