NMR-based metabolomics

382 Pages·2018·15.584 MB·English

by  Keun, Hector C

NMR-based Metabolomics
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New Developments in NMR
Editor-in-chief:
William S. Price, Western Sydney University, Australia
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7- Sharon Ashbrook, University of St Andrews, UK
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7 Bruce Balcom, University of New Brunswick, Canada
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2 István Furó, Industrial NMR Centre at KTH, Sweden
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1 Masatsune Kainosho, Tokyo Metropolitan University, Japan
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9 Maili Liu, Chinese Academy of Sciences, Wuhan, China
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0. Titles in the series:
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doi: 1: Contemporary Computer-Assisted Approaches to Molecular Structure
g | Elucidation
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c. 2: New Applications of NMR in Drug Discovery and Development
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s.r 3: Advances in Biological Solid-State NMR
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p 4: Hyperpolarized Xenon-129 Magnetic Resonance: Concepts, Production,
http:// Techniques and Applications
n 5: Mobile NMR and MRI: Developments and Applications
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uar Design
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0 9: Diffusion NMR of Confined Systems: Fluid Transport in Porous Solids
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d o and Heterogeneous Materials
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12: Cross-relaxation and Cross-correlation Parameters in NMR: Molecular
Approaches
13: Contrast Agents for MRI: Experimental Methods
14: NMR-based Metabolomics
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NMR-based Metabolomics
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or ISSN: 2044-253X
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3 Preface
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0. NMR spectroscopy has long been a leading technique in the study of meta-
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g | and ‘metabonomics’. However, with the advent of metabolic profiling as an
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p:// has been revealed. This is why, despite the superior sensitivity and metab-
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are better rationalised, with a growing understanding of genetic and envi-
ronmental influences. Indeed, this complexity is increasingly embraced as
an advantage, for example, in the study of symbiotic microbes and health
where NMR offers a window into the metabolic cross-talk between multiple
genomes and a myriad of exposures. However, I personally have found that
the most rewarding aspect of using NMR spectroscopy in this context is its
ability to reveal the completely unexpected, sometimes a simple and obvious
but critical observation hidden just out of sight of the investigative team. I
can attest to many projects, laboratory and clinical, rescued by the unique
perspective offered by NMR, and even in today’s world of large-scale studies

New Developments in NMR No. 14
NMR-based Metabolomics
Edited by Hector C. Keun
© The Royal Society of Chemistry 2018
Published by the Royal Society of Chemistry, www.rsc.org
v
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vi Preface
using established methodology, the data generated are continuing to teach
us new and unpredicted things about metabolism.
I salute all the pioneers of the field, cited throughout this volume, for
having the vision and perseverance to realise the potential of the approach,
5 which, in the context of biofluid NMR, is now well on the way to successful
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New Developments in NMR No. 14
NMR-based Metabolomics
Edited by Hector C. Keun
© The Royal Society of Chemistry 2018
Published by the Royal Society of Chemistry, www.rsc.org
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Chapter 2 NMR Pulse Sequences for Metabolomics 22
Bénédicte Elena-Herrmann
2.1 Introduction 22
2.2 Standard 1D NMR Pulses Sequences for
High-throughput Metabolomics 23
2.2.1 One-dimensional 1H NOESY Experiment 23
2.2.2 The Carr–Purcell–Meiboom–Gill (CPMG)
Experiment 25
2.2.3 Diffusion-edited NMR Spectroscopy 25

New Developments in NMR No. 14
NMR-based Metabolomics
Edited by Hector C. Keun
© The Royal Society of Chemistry 2018
Published by the Royal Society of Chemistry, www.rsc.org
ix
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x Contents
2.3 Water and Solvent Suppression for NMR of
Biofluids 27
2.3.1 Water Pre-saturation 27
2.3.2 Advanced Water Suppression Schemes 28
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Metabolomics in Toxicology 43
3.1.3 Analytical Reproducibility of Urine NMR
Spectra 46
3.2 NMR Spectroscopy of Urine in Metabolomics
Studies 48
3.2.1 Collection and Storage of Urine Samples 48
3.2.2 Preparation of Urine Samples for NMR 53
3.2.3 Recommendations Pertaining to Urine
Sample Collection, Storage and Treatment
with a Focus on Diagnostic Study 56
3.2.4 One-dimensional NMR Experiments and
Suppression Methods for Use with Urine 57
3.2.5 Two-dimensional NMR Experiments and
Suppression Methods for Use with Urine 59
3.2.6 Normalization of Urine NMR Spectral
Datasets 60
3.2.7 Multivariate Statistical Analysis of
NMR Urine Spectra 63
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Contents xi
3.3 NMR Spectroscopy of Urine: Systems Biology
Applications 66
3.3.1 Metabolite Variation in Urine from Healthy
Subjects 66
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4.4 Future Perspectives 115
References 116
Chapter 5 High-resolution Magic-angle Spinning (HR-MAS)
NMR Spectroscopy 133
Alan Wong and Covadonga Lucas-Torres
5.1 Introduction 133
5.2 HR-MAS Basic Concepts 134
5.2.1 Magnetic Susceptibility Broadening 134
5.2.2 Magic-angle Spinning 136
5.3 Hardware and Practical Considerations 138
5.3.1 Magnetic Susceptibility Components 138
5.3.2 B Field Correction 138
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5.3.4 Sample Temperature 140
5.3.5 Pulse-field Gradient 140
5.3.6 Pulse Experiments 141