scholarly journals HR-MAS NMR Applications in Plant Metabolomics

Molecules ◽  
2021 ◽  
Vol 26 (4) ◽  
pp. 931
Author(s):  
Dieuwertje Augustijn ◽  
Huub J. M. de Groot ◽  
A. Alia

Metabolomics is used to reduce the complexity of plants and to understand the underlying pathways of the plant phenotype. The metabolic profile of plants can be obtained by mass spectrometry or liquid-state NMR. The extraction of metabolites from the sample is necessary for both techniques to obtain the metabolic profile. This extraction step can be eliminated by making use of high-resolution magic angle spinning (HR-MAS) NMR. In this review, an HR-MAS NMR-based workflow is described in more detail, including used pulse sequences in metabolomics. The pre-processing steps of one-dimensional HR-MAS NMR spectra are presented, including spectral alignment, baseline correction, bucketing, normalisation and scaling procedures. We also highlight some of the models which can be used to perform multivariate analysis on the HR-MAS NMR spectra. Finally, applications of HR-MAS NMR in plant metabolomics are described and show that HR-MAS NMR is a powerful tool for plant metabolomics studies.

1999 ◽  
Vol 77 (11) ◽  
pp. 1962-1972
Author(s):  
Scott Kroeker ◽  
Roderick E Wasylishen

Direct NMR observation of copper-63/65 nuclei in solid K3Cu(CN)4 provides the first experimental example of anisotropic copper chemical shielding. Axially symmetric by virtue of the space group symmetry, the shielding tensor spans 42 ppm, with the greatest shielding when the unique axis is perpendicular to the applied magnetic field. The nuclear quadrupole coupling constant is also appreciable, CQ(63Cu) = -1.125 MHz, reflecting a deviation of the Cu(CN)43- anion from pure tetrahedral symmetry. Spin-spin coupling to 13C nuclei in an isotopically enriched sample is quantified by line-shape simulations of both 13C and 63/65Cu magic-angle spinning (MAS) NMR spectra to be 300 Hz. It is shown that this information is also directly available by 63/65Cu triple-quantum (3Q) MAS NMR. The relative merits of these three approaches to characterizing spin-spin couplings involving half-integer quadrupolar nuclei are discussed. Chemical shielding tensors for nitrogen-15 and carbon-13 are obtained from NMR spectra of non-spinning samples, and are compared to those of tetrahedral group 12 tetracyanometallates. Finally, 2J(63/65Cu,15N) detected in 15N MAS experiments are found to be 19 and 20 Hz for the two crystallographically distinct cyanide ligands.Key words: NMR, quadrupolar nucleus, chemical shielding tensor, multiple-quantum magic-angle spinning, metal cyanide, spin-spin coupling.


The Analyst ◽  
2015 ◽  
Vol 140 (12) ◽  
pp. 3942-3946 ◽  
Author(s):  
Marion André ◽  
Martial Piotto ◽  
Stefano Caldarelli ◽  
Jean-Nicolas Dumez

The acquisition of ultrafast high-resolution magic-angle spinning (HR-MAS) NMR spectra of semi-solid samples is demonstrated.


2003 ◽  
Vol 775 ◽  
Author(s):  
Andrei Nossov ◽  
Flavien Guenneau ◽  
Marie-Anne Springuel-Huet ◽  
Valérie Montouillout ◽  
Jean-Pierre Cognec ◽  
...  

Summary:A Magic Angle Spinning (MAS) NMR probe has been designed allowing the in-situ measurements of NMR spectra of working catalyst. The probe was built following the original design of M. Hunger [Hunger, 1995 #2]. It allows the magic angle spinning of powder samples up to 3.5 kHz, under gas flowing conditions, and at temperatures up to 573K.


1992 ◽  
Vol 7 (7) ◽  
pp. 1892-1899 ◽  
Author(s):  
R.K. Brow ◽  
Z.A. Osborne ◽  
R.J. Kirkpatrick

We have examined the bonding arrangements in Na–P–O–F and Na–Al–P–O–F glasses using 19F, 27Al, and 31P solid-state magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy. For the Al-free series of glasses, the 19F NMR spectra are dominated by peaks near +90 ppm, representative of F terminating P-chains. The formation of these bonds has little effect on the 31P chemical shifts, indicating that F preferentially replaces bridging oxygen on the phosphate tetrahedra, consistent with previous NMR studies of crystalline fluorophosphates and other spectroscopic studies of fluorophosphate glass. For the Na–Al–P–O–F glasses, 27Al NMR detects only octahedral Al-sites, the 19F NMR spectra include a second peak near −12 ppm due to F bonded to Al, and the 31P NMR spectra contain signals due to Q1-sites with one or more Al next-nearest neighbors. The relative intensity of the two 19F peaks correlates well with previous spectroscopic studies and shows that a greater fraction of F–P bonds forms when the base glass is remelted in NH4HF2.


2018 ◽  
Vol 20 (46) ◽  
pp. 29351-29361 ◽  
Author(s):  
V. S. Veena ◽  
Kavya Illath ◽  
Anish Lazar ◽  
C. P. Vinod ◽  
T. G. Ajithkumar ◽  
...  

Proposed model of water layers and pore filling in ethane substituted periodic mesoporous organosilicates (PMOE) based on analysis of solid state magic angle spinning (MAS) proton NMR spectra.


Author(s):  
Caitlin M. Quinn ◽  
Tatyana Polenova

AbstractIn recent years, exciting developments in instrument technology and experimental methodology have advanced the field of magic-angle spinning (MAS) nuclear magnetic resonance (NMR) to new heights. Contemporary MAS NMR yields atomic-level insights into structure and dynamics of an astounding range of biological systems, many of which cannot be studied by other methods. With the advent of fast MAS, proton detection, and novel pulse sequences, large supramolecular assemblies, such as cytoskeletal proteins and intact viruses, are now accessible for detailed analysis. In this review, we will discuss the current MAS NMR methodologies that enable characterization of complex biomolecular systems and will present examples of applications to several classes of assemblies comprising bacterial and mammalian cytoskeleton as well as human immunodeficiency virus 1 and bacteriophage viruses. The body of work reviewed herein is representative of the recent advancements in the field, with respect to the complexity of the systems studied, the quality of the data, and the significance to the biology.


Clay Minerals ◽  
2003 ◽  
Vol 38 (4) ◽  
pp. 551-559 ◽  
Author(s):  
H. P. He ◽  
J . G. Guo ◽  
J . X. Zhu ◽  
C. Hu

AbstractThe thermal transformations of kaolinite have been studied using 27Al and 29Si magic angle spinning nuclear magnetic resonance (MAS NMR), X-ray diffraction (XRD), differential thermal analysis (DTA) and thermogravimetric analysis (TG). The experimental results show that this sample is a pure kaolinite which contains ∼3% carbonaceous material as impurity. 27Al and 29Si MAS NMR spectra show that the microstructural evolution of the thermal transformation of kaolinite at 450 –1050ºC is similar to that of the kaolinite– mullite reaction series previously published by many authors. 29Si MAS NMR spectra of mullite at 1190 and 1250ºC display two resonances at ∼ – 87 and –92 ppm, corresponding to sillimanite-type geometry around Si and the typical Si environment of mullite, respectively. At 1350ºC, the splitting of (hk0) and (kh0) of mullite occurs, indicating that the primary mullite transforms into orthorhombic mullite. Simultaneously, the resonance at ∼ – 92 ppm splits into two signals at ∼ –90 and –94 ppm. 27Al MAS NMR spectra of the mullite consist of three signals centred at ∼ –4, 45 and 60 ppm, corresponding to octahedral, distorted tetrahedral and tetrahedral Al sites, respectively.


2007 ◽  
Vol 361-363 ◽  
pp. 825-828 ◽  
Author(s):  
Fei Wang ◽  
Artemis Stamboulis ◽  
D. Holland ◽  
Shigeki Matsuya ◽  
Akari Takeuchi

The glass based on a 1.5SiO2-Al2O3-0.5P2O5-CaO-0.67CaF2 composition was produced and substituted gradually by barium. The structure of the glasses was studied by multinuclear Magic Angle Spinning Nuclear Magnetic Resonance (MAS-NMR) and Fourier Transform Infrared Spectroscopy (FTIR). It was indicated by 29Si and 31P MAS-NMR spectra that silicon was present as Q4 (4Al) and Q3 (3Al) species and phosphorus was in a Q1 pyrophosphate environment. 29Al MAS-NMR spectra showed that four fold coordinated aluminum Al (IV) was the dominant species with a second peak assigned to octahedral aluminum Al (VI). The 19F spectra suggested that the barium addition caused the formation of Al-F-Ba(n) and F-Ba(n) species. Furthermore, a distribution of silicate network including Si-O-Si stretching (Q4 and Q3) and Si-O-[NBO] (Q3) per SiO4 was reflected by the FTIR study.


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