High-resolution (1)H and (1)H-(13)C magic angle spinning NMR spectroscopy of rat liver.
High-resolution magic angle spinning (MAS) (1)H NMR spectra of small samples (ca. 8 mg) of intact rat liver are reported for the first time. One dimensional spectra reveal a number of large well-resolved NMR signals mainly from low to medium molecular weight compounds (generally <1000 Daltons) from a variety of chemical classes. A range of 2D MAS-NMR experiments were performed, including (1)H J-resolved (JRES), (1)H-(1)H total correlation spectroscopy (TOCSY) and (1)H-(13)C heteronuclear multiple quantum coherence (HMQC) to enable detailed signal assignment. Resonances were assigned from alpha- and beta-glucose, glycerol, alanine, glutamate, glycine, dimethylglycine, lysine, and threonine, together with phosphocholine, choline, lactate, trimethylamine-N-oxide (TMAO), and certain fatty acids. Well-resolved (1)H NMR signals from glycogen (poly 1-4 alpha-glucose) were observed directly in intact liver using MAS-NMR spectroscopy. In addition, the resonances from the glycogen C(1)H proton in alpha(1-->4) linked glucose units with either alpha(1-->4) units adjacent or alpha(1-->6) linked branches could be resolved in a high-resolution (1)H NMR experiment giving direct in situ information on the ratio of alpha(1-->4) to alpha(1-->6) units. This indicates that despite the relatively high MW (>1,000,000 Daltons) there is considerable segmental motion in the glycogen molecules giving long (1)H T(2) relaxation times. Magn Reson Med 44:201-207, 2000.
Biological Chemistry, Biomedical Sciences Division, Imperial College of Science, Technology and Medicine, South Kensington, London, UK.
M E
ME
Bollard
S
S
Garrod
E
E
Holmes
J C
JC
Lindon
E
E
Humpfer
M
M
Spraul
J K
JK
Nicholson
D000818:Animals; D002247:Carbon Isotopes; D006859:Hydrogen; D008099:Liver / Q000378:metabolism*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008297:Male; D051381:Rats
D002247:Carbon Isotopes; D006859:Hydrogen