High-resolution 1H and 1H-13C magic angle spinning NMR spectroscopy of rat liver

High‐resolution magic angle spinning (MAS) 1H 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 1,000,000 Daltons) the...

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Published in:Magnetic resonance in medicine 2000-08, Vol.44 (2), p.201-207
Main Authors: Bollard, M.E., Garrod, S., Holmes, E., Lindon, J.C., Humpfer, E., Spraul, M., Nicholson, J.K.
Format: Article
Language:English
Subjects:
1H MAS NMR
1H-13CMAS NMR
Biological and medical sciences
Digestive system
glycogen
HMQC
Investigative techniques, diagnostic techniques (general aspects)
liver
magic angle spinning
Medical sciences
Radiodiagnosis. Nmr imagery. Nmr spectrometry
rat
TOCSY
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container_end_page 207
container_issue 2
container_start_page 201
container_title Magnetic resonance in medicine
container_volume 44
creator Bollard, M.E.
Garrod, S.
Holmes, E.
Lindon, J.C.
Humpfer, E.
Spraul, M.
Nicholson, J.K.
description High‐resolution magic angle spinning (MAS) 1H 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 1,000,000 Daltons) there is considerable segmental motion in the glycogen molecules giving long 1H T2 relaxation times. Magn Reson Med 44:201–207, 2000. © 2000 Wiley‐Liss, Inc.
doi_str_mv 10.1002/1522-2594(200008)44:2<201::AID-MRM6>3.0.CO;2-5
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One dimensional spectra reveal a number of large well‐resolved NMR signals mainly from low to medium molecular weight compounds (generally &lt;1000 Daltons) from a variety of chemical classes. A range of 2D MAS‐NMR experiments were performed, including 1H J‐resolved (JRES), 1H‐1H total correlation spectroscopy (TOCSY) and 1H‐13C heteronuclear multiple quantum coherence (HMQC) to enable detailed signal assignment. Resonances were assigned from α‐ and β‐glucose, glycerol, alanine, glutamate, glycine, dimethylglycine, lysine, and threonine, together with phosphocholine, choline, lactate, trimethylamine‐N‐oxide (TMAO), and certain fatty acids. Well‐resolved 1H NMR signals from glycogen (poly 1‐4 α‐glucose) were observed directly in intact liver using MAS‐NMR spectroscopy. In addition, the resonances from the glycogen C1H proton in α(1→4) linked glucose units with either α(1→4) units adjacent or α(1→6) linked branches could be resolved in a high‐resolution 1H NMR experiment giving direct in situ information on the ratio of α(1→4) to α(1→6) units. This indicates that despite the relatively high MW (&gt;1,000,000 Daltons) there is considerable segmental motion in the glycogen molecules giving long 1H T2 relaxation times. 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Reson. Med</addtitle><description>High‐resolution magic angle spinning (MAS) 1H 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 &lt;1000 Daltons) from a variety of chemical classes. A range of 2D MAS‐NMR experiments were performed, including 1H J‐resolved (JRES), 1H‐1H total correlation spectroscopy (TOCSY) and 1H‐13C heteronuclear multiple quantum coherence (HMQC) to enable detailed signal assignment. Resonances were assigned from α‐ and β‐glucose, glycerol, alanine, glutamate, glycine, dimethylglycine, lysine, and threonine, together with phosphocholine, choline, lactate, trimethylamine‐N‐oxide (TMAO), and certain fatty acids. Well‐resolved 1H NMR signals from glycogen (poly 1‐4 α‐glucose) were observed directly in intact liver using MAS‐NMR spectroscopy. 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subjects 1H MAS NMR
1H-13CMAS NMR
Biological and medical sciences
Digestive system
glycogen
HMQC
Investigative techniques, diagnostic techniques (general aspects)
liver
magic angle spinning
Medical sciences
Radiodiagnosis. Nmr imagery. Nmr spectrometry
rat
TOCSY
title High-resolution 1H and 1H-13C magic angle spinning NMR spectroscopy of rat liver
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