Arabinoxylan (HBAX-60) was fractioned from alkaline-extracted arabinoxylan (HBAX) in the whole grain of hull-less barley (Hordeum vulgare L. var. nudum Hook. f. Poaceae) by 60% ethanol precipitation, which was studied for physicochemical properties and structure elucidation. Highly purified HBAX-60 mainly composed of arabinose (40.7%) and xylose (59.3%) was created. The methylation and NMR analysis of HBAX-60 indicated that a low-branched β-(1→4)-linked xylan backbone possessed un-substituted (1,4-linked β-Xylp, 36.2%), mono-substituted (β-1,3,4-linked Xylp, 5.9%), and di-substituted (1,2,3,4-linked β-Xylp, 12.1%) xylose units as the main chains, though other residues (α-Araf-(1→, β-Xylp-(1→, α-Araf-(1→3)-α-Araf-(1→ or β-Xylp-(1→3)-α-Araf-(1→) were also determined. Additionally, HBAX-60 exhibited random coil conformation in a 0.1 M NaNO3 solution. This work provides the properties and structural basis of the hull-less barley-derived arabinoxylan, which facilitates further research for exploring the structure–function relationship and application of arabinoxylan from hull-less barley.
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