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The novel highly sulfated (35%) fucoidan fraction  Cf2  , which contained, along with fucose, galactose and traces of xylose and uronic acids was purified from the brown alga  Coccophora langsdorfii . Its structural features were predominantly determined (in comparison with fragments of known structure) by a rapid mass spectrometric investigation of the low-molecular-weight fragments, obtained by “mild” (5 mg/mL) and “exhaustive” (maximal concentration) autohydrolysis. Tandem matrix-assisted laser desorption/ionization mass spectra (MALDI-TOF/TOFMS) of fucooligosaccharides with even degree of polymerization (DP), obtained by “mild” autohydrolysis, were the same as that observed for fucoidan from  Fucus evanescens , which have a backbone of alternating (1 → 3)- and (1 → 4) linked sulfated at C-2 and sometimes at C-4 of 3-linked   α  -L-Fuc p  residues. Fragmentation patterns of oligosaccharides with odd DP indicated sulfation at C-2 and at C-4 of (1 → 3) linked   α  -L-Fuc p  residues on the reducing terminus. Minor sulfation at C-3 was also suggested. The “exhaustive” autohydrolysis allowed us to observe the “mixed” oligosaccharides, built up of fucose/xylose and fucose/galactose. Xylose residues were found to occupy both the reducing and nonreducing termini of FucXyl disaccharides. Nonreducing galactose residues as part of GalFuc disaccharides were found to be linked, possibly, by 2-type of linkage to fucose residues and were found to be sulfated, most likely, at position C-2.

Rapid Mass Spectrometric Analysis of a Novel Fucoidan, Extracted from the Brown AlgaCoccophora langsdorfii