Synthesis and analysis of electrospray ionization-generated five-coordinate diastereomeric Ni-N-glycoside complexes using a quadrupole ion trap mass spectrometer
G. Smith et Ja. Leary, Synthesis and analysis of electrospray ionization-generated five-coordinate diastereomeric Ni-N-glycoside complexes using a quadrupole ion trap mass spectrometer, INT J MASS, 193(2-3), 1999, pp. 153-160
Five-coordinate Ni N-glycoside complexes, consisting of a single tridentate
N-glycoside ligand and a bidentate day ligand coordinated to a central Ni(
II) ion, were synthesized for a series of diastereomeric monosaccharides. F
ollowing excitation of the precursor ions in a quadrupole ion trap, reprodu
cibly distinct product ion spectra were obtained for each diastereomeric co
mplex. Neutral losses resulted from cross-ring cleavages of the monosacchar
ide ring and/or losses of a bidentate day ligand. Isotopic labeling studies
confirmed which particular carbon centers were lost from the precursor ion
as a result of the: cross-ring cleavages. Synthesis of the Ni-N glycoside
complex was achieved using as little as 21 mu g of monosaccharide. Producti
on of the representative five-coordinate precursor ion was obtained over a
wide range of metal-ligand:monosaccharide molar ratios and product ion spec
tra remained reproducible over this range. (C) 1999 Elsevier Science B.V.