A new gradient-controlled method for improving the spectral width of ultrafast 2D NMR experiments

Giraudeau, Patrick; Akoka, Serge

doi:10.1016/j.jmr.2010.05.002

Cited by 41 publications

(10 citation statements)

References 33 publications

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“…The simulation was carried out with T 2 ¼ 300 ms and a diffusion coefficient D ¼ 2.3 Â 10 À9 m 2 /s. In 2010, we described a slightly less efficient, but much more general approach for folding resonances in the ultrafast dimension (Giraudeau & Akoka, 2010). Similar results are obtained for other spatial-encoding schemes.…”

Section: State-of-the-art In Improving the Quality Of Ultrafast Expersupporting

confidence: 60%

Fast and Ultrafast Quantitative 2D NMR

Giraudeau

Akoka

2013

Advances in Botanical Research

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Section: State-of-the-art In Improving the Quality Of Ultrafast Expersupporting

confidence: 60%

Fast and Ultrafast Quantitative 2D NMR

Giraudeau

Akoka

2013

Advances in Botanical Research

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“…On the other hand, the NMR community has developed a number of approaches departing from the classical parametric incrementation scheme of 2D NMR, in order to drastically reduce the duration of 2D NMR experiments. − In particular, the last 10 years have witnessed large efforts geared at developing the so-called “ultrafast 2D NMR” methodology, ,, capable of providing a complete 2D correlation in a single scan, i.e., in a fraction of a second. It relies on a spatial-encoding procedure over the sample length which has been described in detail in recent papers. − This methodology initially suffered from important limitations in terms of resolution and sensitivity, − but over the past few years, several significant improvements have increased its analytical performance, − making it suitable for the quantitative analysis of complex mixtures. , These first quantitative applications of ultrafast 2D NMR naturally raised the question of how such spatially encoded approaches would compare to conventional 2D NMR in terms of analytical performance. Sensitivity issues should be particularly taken into consideration when dealing with biological mixtures such as those involved in metabolomic studies.…”

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confidence: 99%

Fast Determination of Absolute Metabolite Concentrations by Spatially Encoded 2D NMR: Application to Breast Cancer Cell Extracts

et al. 2012

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Two-dimensional nuclear magnetic resonance (2D NMR) forms a powerful tool for the quantitative analysis of complex mixtures such as samples of metabolic relevance. However, its use for quantitative purposes is far from being trivial, not only because of the associated experiment time, but also due to its subsequent high sensitivity to hardware instabilities affecting its precision. In this paper, an alternative approach is considered to measure absolute metabolite concentrations in complex mixtures with a high precision in a reasonable time. It is based on a "multi-scan single shot" (M3S) strategy, which is derived from the ultrafast 2D NMR methodology. First, the analytical performance of this methodology is compared to the one of conventional 2D NMR. 2D correlation spectroscopy (COSY) spectra are obtained in 10 min on model metabolic mixtures, with a precision in the 1-4% range (versus 5-18% for the conventional approach). The M3S approach also shows a better linearity than its conventional counterpart. It ensures that accurate quantitative results can be obtained provided that a calibration procedure is carried out. The M3S COSY approach is then applied to measure the absolute metabolite concentration in three breast cancer cell line extracts, relying on a standard addition protocol. M3S COSY spectra of such extracts are recorded in 20 min and give access to the absolute concentration of 14 major metabolites, showing significant differences between cell lines.

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“…A far more significant breakthrough was reported in 2002 by L. Frydman and co-workers, who proposed a revolutionary approach capable of providing a complete 2D correlation in a single scan, i.e., in a fraction of a second . This “ultrafast 2D NMR” methodology initially suffered from important limitations in terms of resolution and sensitivity, − but over the past few years, several significant methodological improvements have brought substantial improvements to this technique, ,− making it suitable for analyzing mixtures with increasing complexity. Moreover, we showed recently that ultrafast 2D NMR formed a valuable tool for precise quantitative analysis .…”

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Ultrafast Quantitative 2D NMR: An Efficient Tool for the Measurement of Specific Isotopic Enrichments in Complex Biological Mixtures

et al. 2011

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Two-dimensional nuclear magnetic resonance (2D NMR) is a promising tool for studying metabolic fluxes by measuring (13)C-enrichments in complex mixtures of (13)C-labeled metabolites. However, the methods reported so far are hampered by very long acquisition durations limiting the use of 2D NMR as a quantitative tool for fluxomics. In this paper, we propose a new approach for measuring specific (13)C-enrichments in a very fast way, by using new experiments based on ultrafast 2D NMR. Two homonuclear 2D experiments (ultrafast COSY and zTOCSY) are proposed to measure (13)C-enrichments in a single scan. Their advantages and limitations are discussed, and their high analytical potentialities are highlighted. Both methods are characterized by an accuracy of 1-2%, an average precision of 3%, and an excellent linearity. The analytical performance is equivalent or better than any of the conventional methods previously reported. The two ultrafast experiments are applied to the measurement of (13)C-enrichments on a biomass hydrolyzate, showing the first known application of ultrafast 2D NMR to a real biological extract. The experiment duration is divided by 200 compared to the conventional methods, while preserving 80% of the quantitative information. This new approach opens new perspectives of application for fluxomics and metabonomics.

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A new gradient-controlled method for improving the spectral width of ultrafast 2D NMR experiments

Cited by 41 publications

References 33 publications

Fast and Ultrafast Quantitative 2D NMR

Fast and Ultrafast Quantitative 2D NMR

Fast Determination of Absolute Metabolite Concentrations by Spatially Encoded 2D NMR: Application to Breast Cancer Cell Extracts

Ultrafast Quantitative 2D NMR: An Efficient Tool for the Measurement of Specific Isotopic Enrichments in Complex Biological Mixtures

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