Inferences on the nature of a Cr(V) or Cr(IV) species formed by reduction of dichromate by a bovine liver homogenate: NMR and mass-spectrometric studies.
A low-molecular weight chromium-containing fraction of the material resulting from dichromate reduction by bovine liver homogenate was investigated by NMR and ES-MS. The ES-MS spectrum showed a readily detectable peak at m/z = 786.1. The same molecular weight reasonably agreed with the relatively low diffusion coefficient measured by NMR-DOSY experiments on the main species observed in the (1)H NMR spectrum. At least two downfield shifted and broad paramagnetic signals were apparent in the (1)H NMR spectrum. Temperature dependence of chemical shift was exploited in order to estimate the diamagnetic shift of the signals in the diamagnetic region of the spectrum. 2D TOCSY, NOESY, COSY and (1)H-(3)C HMQC spectra revealed the presence of aromatic protons (which were assigned as His residues), Gly and some other short chain amino-acids. Combinations of the molecular masses of such components together with acetate (which is present in the solution) and chromium atoms allowed a tentative proposal of a model for the compound.
Gaggelli
Elena
E
Department of Chemistry University of Siena Via A.Moro Siena 53100 Italy.
D'Amelio
Nicola
N
Gaggelli
Nicola
N
Valensin
Gianni
G
Bovalini
Lucia
L
Paffetti
Alessandro
A
Trabalzini
Lorenza
L