Chondroitin sulfates were fragmented using the enzymes chondroitin sulfate ABC endolyase and chondroitin ACII lyase; both disaccharide and tetrasaccharide fragments were isolated after reduction to the corresponding 2-deoxy-2-N-acetylamino-d-galactitol (GalNAc-ol) form. These have the structures: ΔUA(β1–3)GalNAc4S-ol, ΔUA(β1–3)GalNAc6S-ol, ΔUA2S(β1–3)GalNAc6S-ol, ΔUA(β1–3)GalNAc4S(β1–4)l-IdoA(α1–3)GalNAc4S-ol, ΔUA(β1–3)GalNAc4S(β1–4)GlcA(β1–3)GalNAc4S-ol, ΔUA(β1–3)GalNAc6S(β1–4)GlcA(β1–3)GalNAc4S-ol, ΔUA(β1–3)GalNAc6S(β1–4)GlcA(β1–3)GalNAc6S-ol, ΔUA2S(β1–3)GalNAc6S(β1–4)GlcA(β1–3)GalNAc4S-ol and ΔUA2S(β1–3)GalNAc6S(β1–4)GlcA(β1–3)GalNAc6S-ol, where ΔUA represents a 4,5-unsaturated hexuronic acid (4-deoxy-α-lthreo-hex-4-enepyranosyluronic acid) and 6S/4S/2S represent O-ester sulfate groups at C6/C4/C2 sites. Complete 1H-NMR and 13C-NMR data are derived for these species, which may help to alleviate some of the significant difficulties resulting from signal complexity that are currently hindering the characterization and assignment of major and minor structural components within chondroitin sulfate and dermatan sulfate polymers.