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Title: Biophysical applications of solid state and tritium NMR

Technical Report ·
OSTI ID:5640898

Novel applications of Magic Angle Sample Spinning (MASS) and Tritium (/sup 3/H) NMR to the study of mammalian tissue and in vivo metabolism, respectively, are described. The solid state /sup 31/P MASS NMR spectra of sodium, magnesium, and calcium complexes of adenosine triphosphate (ATP) were recorded. These spectra indicate that the terminal phosphate group of the sodium complex is protonated in contrast to the unprotonated divalent complexes. The chemical shift tensors of a large variety of phosphates and phosphate esters were measured. The magnitude of the sigma/sub 33/, the low field, elements of the /sup 31/P chemical shift tensors in these phosphates were linearly related to the longest P-O bonds and the sigma/sub 11/, the high field, elements to the shortest bonds. Similar relationships were found when these tensor elements were plotted against bond angles. The implications of these observations are discussed in the context of phosphorus-oxygen d-p ..pi.. bonding interactions. /sup 31/P and /sup 1/H MASS NMR were applied to the study of lyophilized rat tissue. The /sup 31/P spectra exhibit resonances from phospholipids, DNA, ATP and NAD. The MASS results were compared to chemical analysis data obtained by others and to calculated spectra based on MASS data of model compounds. The /sup 1/H MASS spectra of these tissue samples exhibited lines with widths less than 40 Hz, and were assigned to phospholipid protons. The intensity distribution of the /sup 1/H spectra supported this assignment. Motionally narrowed /sup 31/P and /sup 1/H resonances suggest that the phospholipids undergo varying degrees of motion with correlation times ranging from 0.5 ns to 2 ..mu..s. The degree of hydration of the DNA was also established. 100 refs.

Research Organization:
Lawrence Berkeley Lab., CA (USA)
DOE Contract Number:
AC03-76SF00098
OSTI ID:
5640898
Report Number(s):
LBL-24384; ON: DE88005328
Resource Relation:
Other Information: Thesis (Ph.D.). Portions of this document are illegible in microfiche products
Country of Publication:
United States
Language:
English

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