GLYCOSYL COMPOSITION OF COLLAGENS

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NMR analysis was performed on a Varian Inova 600-MHz spectrometer. The sample was deuterium-exchanged by lyophilization from D2O and dissolved in 0.5 mL D2O. The 1H-NMR 1-D and 2-D TOCSY (total correlation spectroscopy), 13C-1H-HSQC (heteronuclear single quantum correlation), and -HMBC (heteronuclear multiple-bond correlation) spectra were acquired at 25(C. Proton chemical shifts were measured relative to internal acetone standard. The 1-D 1H-NMR spectral data were comparable to those published previously for an oligosaccharide fragment identical in structure to that proposed for this sample. The monosaccharide sequence and linkage structure were confirmed by a series of 1H-1H-homonuclear (TOCSY) and 13C-1H-heteronuclear correlation experiments (HSQC, HMBC).