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Identifying unknown metabolites using NMR-based metabolic profiling techniques
Journal article   Peer reviewed

Identifying unknown metabolites using NMR-based metabolic profiling techniques

I. Garcia-Perez, J.M. Posma, J.I. Serrano-Contreras, C.L. Boulangé, Q. Chan, G. Frost, J. Stamler, P. Elliott, J.C. Lindon, E. Holmes, …
Nature Protocols, Vol.15, pp.2538-2567
2020
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Abstract

Metabolic profiling of biological samples provides important insights into multiple physiological and pathological processes but is hindered by a lack of automated annotation and standardized methods for structure elucidation of candidate disease biomarkers. Here we describe a system for identifying molecular species derived from nuclear magnetic resonance (NMR) spectroscopy-based metabolic phenotyping studies, with detailed information on sample preparation, data acquisition and data modeling. We provide eight different modular workflows to be followed in a recommended sequential order according to their level of difficulty. This multi-platform system involves the use of statistical spectroscopic tools such as Statistical Total Correlation Spectroscopy (STOCSY), Subset Optimization by Reference Matching (STORM) and Resolution-Enhanced (RED)-STORM to identify other signals in the NMR spectra relating to the same molecule. It also uses two-dimensional NMR spectroscopic analysis, separation and pre-concentration techniques, multiple hyphenated analytical platforms and data extraction from existing databases. The complete system, using all eight workflows, would take up to a month, as it includes multi-dimensional NMR experiments that require prolonged experiment times. However, easier identification cases using fewer steps would take 2 or 3 days. This approach to biomarker discovery is efficient and cost-effective and offers increased chemical space coverage of the metabolome, resulting in faster and more accurate assignment of NMR-generated biomarkers arising from metabolic phenotyping studies. It requires a basic understanding of MATLAB to use the statistical spectroscopic tools and analytical skills to perform solid phase extraction (SPE), liquid chromatography (LC) fraction collection, LC-NMR-mass spectroscopy and one-dimensional and two-dimensional NMR experiments.

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Collaboration types
Domestic collaboration
International collaboration
Citation topics
2 Chemistry
2.211 Mass Spectrometry
2.211.990 Metabolomics
Web Of Science research areas
Biochemical Research Methods
ESI research areas
Biology & Biochemistry
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