Arabinoxylan-derived oligosaccharides were treated with (1-->4)-beta-D-arabinoxylan arabinofuranohydrolase (AXH) and two types of alpha-L-arabinofuranosidase, A and B. Analysis of reaction products by high performance anion-exchange chromatography indicated the removal of arabinofuranosyl groups from singly substituted xylopyranosyl residues. In addition, differences in the specificity of these enzymes towards the various differently substituted oligosaccharides were observed. 1H NMR spectroscopy and methylation analysis of alkali-extractable wheat-flour arabinoxylan treated with AXH confirmed the specificity of AXH towards (1-->3)-linked arabinofuranosyl groups on singly substituted xylopyranosyl residues. With these techniques, alpha-L-arabinofuranosidase B was found to cause minor changes in (1-->2)- and (1-->3)-linked arabinofuranosyl groups on doubly substituted xylopyranosyl residues.