Ultrahigh‐Resolution Diffusion‐Ordered Spectroscopy

Foroozandeh, Mohammadali; Castañar, Laura; Martins, Lucas G.; Sinnaeve, Davy; Tormena, Cláudio F.; Adams, Ralph W.; Poggetto, Guilherme Dal; Nilsson, Mathias

doi:10.1002/ange.201609676

Cited by 17 publications

(16 citation statements)

References 54 publications

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“…PSYCHE-iDOSY is a unique pseudo 3D method involving the combination of a diffusion dimension with PSYCHE pure shift. 22,23 Despite being invented in 2016, PSYCHE-iDOSY has not yet been exploited for the analysis of pyrolysis oils. 24 Both PSYCHE and DOSY experiments combined have the capability to verify signals from the 1D 1H spectrum as belonging to a specific component, which can then be quantified using software such as Chenomx NMR Suite TM .…”

Section: Pure Shiftmentioning

confidence: 99%

Application of pure shift and diffusion NMR for the characterisation of crude and processed pyrolysis oil

Gresley

Broadberry

Robertson

et al. 2019

Journal of Analytical and Applied Pyrolysis

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HighlightsDiffusion NMR used to characterise molecular mass distribution of pyrolysis oil components.PSYCHE-iDOSY experiments acquired on pyrolysis oil for the first time.Semi-automatic characterisation of water-soluble components using Chenomx™ Abstract By combining diffusion-ordered NMR spectroscopy (DOSY) and pure shift NMR spectroscopy ((Pure Shift Yielded By Chirp Excitation (PSYCHE)) with 1D NMR metabolite assignment, we demonstrate an improved method for in situ analysis of pre and post-processed pyrolysis oil to quickly establish the most effective upgrading 3 procedure. These experiments use molecular mass estimations from DOSY and single component verification using PSYCHE to confirm the identity of metabolites and show how the mass pattern for pyrolysis oils varies depending on how it is upgraded.With the use of a semi-automatic approach for metabolite assignment, we have verified and quantified individual components, giving rise to a collection of potential 'marker compounds'; their changes in concentration being correlated to the upgrading process a pyrolysis oil undergoes.

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Section: Pure Shiftmentioning

confidence: 99%

Application of pure shift and diffusion NMR for the characterisation of crude and processed pyrolysis oil

Gresley

Broadberry

Robertson

et al. 2019

Journal of Analytical and Applied Pyrolysis

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“…The major advantage of PSYCHE is that it is most sensitive among the existing pure shift methods. Several further developments are achieved to obtain ultraclean artifact-free spectra and applied in 2D NMR as well [133,134]. Very recently one such modification named SAPPHIRE-PSYCHE methodology is applied for plant metabolomics study.…”

Section: Pure Shift Nmrmentioning

confidence: 99%

New Advances in Fast Methods of 2D NMR Experiments

Emwas¹,

Alghrably²,

Al-Harthi³

et al. 2020

Nuclear Magnetic Resonance

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Although nuclear magnetic resonance spectroscopy is a potent analytical tool for identification, quantification, and structural elucidation, it suffers from inherently low sensitivity limitations. This chapter focuses on recently reported methods that enable quick acquisition of NMR spectra, as well as new methods of faster, efficient, and informative two-dimensional (2D) NMR methods. Fast and efficient data acquisition has risen in response to an increasing need to investigate chemical and biological processes in real time. Several new techniques have been successfully introduced. One example of this is band-selective optimized-flip-angle shorttransient (SOFAST) NMR, which has opened the door to studying the kinetics of biological processes such as the phosphorylation of proteins. The fast recording of NMR spectra allows researchers to investigate time sensitive molecules that have limited stability under experimental conditions. The increasing awareness that molecular structures are dynamic, rather than static, has pushed some researchers to find alternatives to standard, time-consuming methods of 15 N relaxation observables acquisition.Keywords: NMR, 2D NMR, ultrafast data processing, SOFAST, relaxation 15 N, 29 Si, 30 Al, 31 P to 235 U). As the resonating frequency is unique for each type of nuclei, one can envision an NMR for each nucleus as a separate spectroscopy such as 1 H NMR spectroscopy, 13 C NMR spectroscopy, 235 U NMR spectroscopy (Figure 1), etc. More importantly, NMR has the ability to evaluate information about the environment of each atom and their neighbor's nuclei (both through space and through bond), allowing researchers to differentiate the unique magnetic environments of the same nuclei in different positions of a single molecule. Thus, NMR spectroscopy is extensively used for the identification and in the structural elucidation in a wide Nuclear Magnetic Resonance 2 range of applications in gas [2,3], liquid [4][5][6][7][8][9][10][11][12][13][14][15][16], and solid-state samples [17][18][19][20][21][22][23][24][25][26][27][28]. Nowadays, NMR spectroscopy is one of the most important analytical tools that has been used in several fields. These fields include structural biology [29][30][31][32][33][34][35][36][37][38], organic chemistry [39][40][41][42][43][44][45][46][47][48][49][50][51][52], polymer characterization [40,46,[53][54][55][56][57][58][59][60][61][62][63][64], inorganic chemistry [65][66][67][68][69][70][71][72][73][74][75], and physics [76][77][78][79][80][81][82][83].Despite its significant advantages, NMR suffers from some limitations, of which the relatively low sensitivity seems to be the most severe. An NMR sample can be treated as a collection of many nuclear spins of magnetically active nuclei that act as small bar magnets. These nuclear spins have two possible orientations with different energy levels that adapt when placed within the strong magnetic field. The number of nuclear spins occupying each energy level is determined by the Boltzmann distribution equation: N ...

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“…In applications with many samples, for example from a large cohort of individuals, strong positive statistical correlations of the changes of peak intensities can be utilized for the assignment of multiple peaks to the same molecule by statistical total correlation spectroscopy (STOCSY) or ratio analysis NMR spectroscopy (RANSY) . For simple mixtures, variations of translational diffusion measured for different NMR peaks by Diffusion‐Ordered Spectroscopy (DOSY) experiments help their attribution to separate molecules …”

Section: Figurementioning

confidence: 99%

Differential Attenuation of NMR Signals by Complementary Ion‐Exchange Resin Beads for De Novo Analysis of Complex Metabolomics Mixtures

Zhang

Yuan

Brüschweiler

2017

Chemistry A European J

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A primary goal of metabolomics is the characterization of a potentially very large number of metabolites that are part of complex mixtures. Application to biofluids and tissue samples offers insights into biochemical metabolic pathways and their role in health and disease. 1D H and 2D C- H HSQC NMR spectra are most commonly used for this purpose. They yield quantitative information about each proton of the mixture, but do not tell which protons belong to the same molecule. Interpretation requires the use of NMR spectral databases, which naturally limits these investigations to known metabolites. Here, a new method is presented that uses complementary ion exchange resin beads to differentially attenuate 2D NMR cross-peaks that belong to different metabolites. Based on their characteristic attenuation patterns, cross-peaks could be clustered and assigned to individual molecules, including unknown metabolites with multiple spin systems, as demonstrated for a metabolite model mixture and E. coli cell lysate.

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Ultrahigh‐Resolution Diffusion‐Ordered Spectroscopy

Abstract: Supportinginformation and the ORCID identification number(s) for the author(s) of this article can be found under: http://dx.

Cited by 17 publications

References 54 publications

Application of pure shift and diffusion NMR for the characterisation of crude and processed pyrolysis oil

Application of pure shift and diffusion NMR for the characterisation of crude and processed pyrolysis oil

New Advances in Fast Methods of 2D NMR Experiments

Differential Attenuation of NMR Signals by Complementary Ion‐Exchange Resin Beads for De Novo Analysis of Complex Metabolomics Mixtures

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