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Complete assignment of the 13C NMR spectra of bleomycin A2 and its zinc complex by means of two-dimensional NMR spectroscopy

✍ Scribed by M. A. J. Akkerman; C. A. G. Haasnoot; U. K. Pandit; C. W. Hilbers

Publisher: John Wiley and Sons
Year: 1988
Tongue: English
Weight: 757 KB
Volume: 26
Category: Article
ISSN: 0749-1581
DOI: 10.1002/mrc.1260260911

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✦ Synopsis

13C NMR spectra of free bleomycin A, at pH 4 and 6.7 and of its zinc complex at pH 6.7 were completely assigned by making use of two-dimensional 'H-"C correlated spectroscopy. Differences in resonance positions between the spectra of the free bleomycin at pH 4 and 6.7 are observed for the /?-hydroxyhistidine and the /?aminoalanine residues, obviously because of protonation/deprotonation of these moieties in the pH region considered. Also, shifts are observed for the carbon resonances of the gulose residue. Upon complex formation between zinc(I1) and bleomycin large 13C shifts are observed for the carbon atoms in the pyrimidinepropionamide, /?hydroxyhistidine, /?-aminoalanine, a-L-gulose and a-D-mannose fragments. Although for some residues the observed shifts correspond with the position of the zinc(1I) binding sites in bleoinycin proposed on the basis of earlier 'H NMR experiments, a simple correlation between the location of the zinc(I1) binding sites and the shifts cannot be drawn.

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