Journal of Lipid Research, Vol 31, 479-486, Copyright © 1990 by Lipid Research, Inc.
31P NMR of phospholipid glycerol phosphodiester residues
TE Merchant and T Glonek
Magnetic Resonance Laboratory, Chicago College of Osteopathic Medicine, IL 60615.
Saponification of extracted tissue phospholipids yields a set of isolated
glycerol 3-phosphoryl phospholipid polar headgroups from which
semi-quantitative 31P NMR spectra can be obtained. The resonance signals
from these molecules, which frequently have been reported as
uncharacterized phosphate signals observed in perchloric acid extracts of
tissue, can be used as an aid in the characterization of isolated
phospholipids and of tissue phospholipid 31P NMR profiles. 31P NMR
chemical-shift values of the resonances at pH 7 in water and relative to
85% phosphoric acid are: glycerol 3-phosphocholine (-0.13 delta), glycerol
3-phosphoethanolamine (0.42 delta), glycerol 3-
phospho(monomethyl)ethanolamine (0.29 delta), glycerol 3-
phospho(dimethyl)ethanolamine (0.16 delta), glycerol 3-phosphoserine (0.14
delta), glycerol 3-phosphoinositol (-0.07 delta), glycerol 3-
phosphoglycerol (0.92 delta), bis(glycerol 3-phospho)glycerol (0.79 delta),
serine ethanolamine phosphodiester (-0.46 delta), glycerol 3- phosphate
(0.60 delta; 4.29 delta at pH 10) glycerol 2-phosphate (0.15 delta; 3.92
delta at pH 10). In addition, analysis of extracted cancer tissue
phospholipid samples yielded a new and uncharacterized polar headgroup
fragment with a chemical-shift value of 0.29 delta that is independent of
sample pH.
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