Fast and precise quantitative analysis of metabolic mixtures by 2D 1H INADEQUATE NMR

Quantitative analysis of metabolic mixtures by 1H 1D NMR offers a limited potential for precise quantification of biomarkers, due to strong overlap between the peaks. Two-dimensional spectroscopy is a powerful tool to unambiguously and simultaneously measure a larger number of metabolite contributio...

Full description

Saved in:
Bibliographic Details
Published in:Journal of pharmaceutical and biomedical analysis 2011-01, Vol.54 (1), p.252-257
Main Authors: Martineau, Estelle, Giraudeau, Patrick, Tea, Illa, Akoka, Serge
Format: Article
Language:English
Subjects:
2D NMR
Analysis
Analytical, structural and metabolic biochemistry
Biological and medical sciences
biomarkers
Biomarkers - chemistry
Buffers
Calibration
Cell Line, Tumor
Chemistry Techniques, Analytical
Chemistry, Pharmaceutical - methods
Fundamental and applied biological sciences. Psychology
General pharmacology
Humans
Hydrogen-Ion Concentration
INADEQUATE
Magnetic Resonance Spectroscopy - methods
Medical sciences
Metabolites
Metabolomics - methods
nuclear magnetic resonance spectroscopy
Pharmacology. Drug treatments
Precision
Quantitative analysis
Reproducibility of Results
Temperature
Time Factors
Citations: Items that this one cites
Items that cite this one
Online Access:Get full text
Tags: Add Tag
No Tags, Be the first to tag this record!
Description
Summary:Quantitative analysis of metabolic mixtures by 1H 1D NMR offers a limited potential for precise quantification of biomarkers, due to strong overlap between the peaks. Two-dimensional spectroscopy is a powerful tool to unambiguously and simultaneously measure a larger number of metabolite contributions. However, it is still rarely used for quantification, first because quantitative analysis by 2D NMR requires a calibration procedure due to the multi-impulsional nature of 2D NMR experiments, and above all because of the prohibitive experiment duration that is necessary to obtain such a calibration curve. In this work, we develop and evaluate a 2D 1H INADEQUATE protocol for a fast determination of metabolite concentrations in complex mixtures. The 2D pulse sequence is carefully optimized and evaluated in terms of precision and linearity. Quantitative 1H INADEQUATE 2D spectra of metabolic mixtures are obtained in 7 min with a repeatability better than 2% for metabolite concentrations as small as 100 μM and an excellent linearity. The method described in this work allows a fast and precise quantification of metabolic mixtures, and it forms a promising tool for metabonomic studies.
ISSN:0731-7085
1873-264X
DOI:10.1016/j.jpba.2010.07.046