scholarly journals Comparison of Regular, Pure Shift, and Fast 2D NMR Experiments for Determination of the Geographical Origin of Walnuts

Metabolites ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 39
Author(s):  
Stephanie Watermann ◽  
Caroline Schmitt ◽  
Tobias Schneider ◽  
Thomas Hackl
Keyword(s):  
Statistical Analysis ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Geographical Origin ◽  
Nuclear Overhauser Effect ◽  
Juglans Regia ◽  
2D Nmr ◽  
Support Vector ◽  
Nuclear Overhauser ◽  
The One

1H NMR spectroscopy, in combination with chemometric methods, was used to analyze the methanol/acetonitrile (1:1) extract of walnut (Juglans Regia L.) regarding the geographical origin of 128 authentic samples from different countries (France, Germany, China) and harvest years (2016–2019). Due to the large number of different metabolites within the acetonitrile/methanol extract, the one-dimensional (1D) 1H NOESY (nuclear Overhauser effect spectroscopy) spectra suffer from strongly overlapping signals. The identification of specific metabolites and statistical analysis are complicated. The use of pure shift 1H NMR spectra such as PSYCHE (pure shift yielded by chirp excitation) or two-dimensional ASAP-HSQC (acceleration by sharing adjacent polarization-heteronuclear single quantum correlation) spectra for multivariate analysis to determine the geographical origin of foods may be a promising method. Different types of NMR spectra (1D 1H NOESY, PSYCHE, and ASAP-HSQC) were acquired for each of the 128 walnut samples and the results of the statistical analysis were compared. A support vector machine classifier was applied for differentiation of samples from Germany/China, France/Germany, and France/China. The models obtained by conduction of a repeated nested cross-validation showed accuracies from 58.9% (±1.3%) to 95.9% (±0.8%). The potential of the 1H-13C HSQC as a 2D NMR experiment for metabolomics studies was shown.

1H NMR studies of [N-MeAib1, Tyr(Me)4]ANGII and [N-MeAib1, Tyr(Me)4, Ile8]ANGII in dimethylsulfoxide by nuclear Overhauser effect (NOE) enhancement spectroscopy: cis-trans Isomerism of the His-Pro bond

1990 ◽  
Vol 55 (4) ◽  
pp. 1106-1111 ◽  
Author(s):  
John Matsoukas ◽  
Paul Cordopatis ◽  
Raghav Yamdagni ◽  
Graham J. Moore
Keyword(s):  
1H Nmr ◽  
Nuclear Overhauser Effect ◽  
Nmr Studies ◽  
Restricted Rotation ◽  
Overhauser Effect ◽  
Major Isomer ◽  
Conformational Properties ◽  
Nuclear Overhauser

The conformational properties of the Sarmesin analogues [N-MeAib1, Tyr(Me)4]ANGII and [N-MeAib1, Tyr(Me)4, Ile8]ANGII in hexadeutero-dimethysulfoxide were investigated by Nuclear Overhauser Effect (NOE) Enhancement Studies. Cis-trans isomers (ratio 1 : 6) due to restricted rotation of the His-Pro bond were observed. Interresidue interactions between the His Cα proton and the two Pro Cδ protons revealed that the major isomer was the trans.

scholarly journals Benderamide A, a Cyclic Depsipeptide from a Singapore Collection of Marine Cyanobacterium cf. Lyngbya sp.

Marine Drugs ◽  
2018 ◽  
Vol 16 (11) ◽  
pp. 409 ◽  
Author(s):  
Chi Ding ◽  
Ji Ong ◽  
Hui Goh ◽  
Cynthia Coffill ◽  
Lik Tan
Keyword(s):  
Breast Cancer Cells ◽  
Nuclear Overhauser Effect ◽  
2D Nmr ◽  
Marine Cyanobacterium ◽  
One Dimensional ◽  
Mechanistic Pathway ◽  
Overhauser Effect ◽  
Cyclic Depsipeptide ◽  
Nuclear Overhauser ◽  
Related Compounds

Benderamide A (1), a (S)-2,2-dimethyl-3-hydroxy-7-octynoic acid (S-Dhoya)-containing cyclic depsipeptide that belongs to the kulolide superfamily, was isolated from a Singapore collection of cf. Lyngbya sp. marine cyanobacterium using a bioassay-guided approach. While the planar structure of 1 was elucidated using a combination of 1D and 2D NMR experiments and MS analysis, the absolute configuration was subsequently achieved using the results obtained from Marfey’s analysis, comparative analysis of nuclear overhauser effect spectroscopy (NOESY) with the known compound 3, and one dimensional-nuclear overhauser effect (1D-NOE). Although 1 did not display antiproliferative activity against MCF7 breast cancer cells, the presence of an Ala instead of Gly suggests a possible mechanistic pathway to explain the consequential decrease in cytotoxicity compared to the closely related 2. In addition, results obtained from an LC–MS/MS-based molecular networking algorithm revealed two other closely related compounds encouraging further identification and isolation from the same marine cyanobacterium extract.

NMR study of heterogeneity in pyridine-N-oxide...HCl crystal

Open Physics ◽  
2004 ◽  
Vol 2 (1) ◽  
Author(s):  
Vytautas Balevicius ◽  
Alexandar Gacesa ◽  
Janez Plavec
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Solid Phase ◽  
Mixing Time ◽  
Exchange Process ◽  
2D Nmr ◽  
Spin Coupling ◽  
Nmr Study ◽  
2D Nmr Spectra ◽  
Heterogeneous Phase

AbstractAn origin of narrow 1H NMR signals in pyridine-N-oxide (PyO)...HCl crystal has been investigated by means of MAS, SPEDAS, NOESY and COSY techniques. Spectra of crystalline samples are compared with those of solid phase obtained from liquid PyO...HCl solutions (in acetonitile/H2O) after the heterogeneous phase separation. It has been concluded that partially resolved peaks in 1H NMR spectra of solids are related with heterogeneity of spin system and presence of different H-bond clusters of water molecules. NOESY spectra show no cross-peaks even at very long mixing time (500 ms). This indicates there is no exchange process between spins causing different peaks, and thus the corresponding molecular aggregates are captured in “islands of mobility8 without any channels sufficient for exchange. Appearance of MAS side bands as “pseudo8 cross-peaks in 2D NMR spectra using MAS/COSY technique is reported. In the case of accidental coincidence of spinning frequency (ωMAS) with spectral distances between some diagonal signals, intensive non-diagonal peaks are observed at the corresponding cross-positions. A misleading conclusion concerning spin coupling is easy to avoid using various ωMAS.

Microstructural study of cetyltrimethylammonium bromide / 1-butanol / salt / water system — SANS and 2D-NOESY analysis

2012 ◽  
Vol 90 (3) ◽  
pp. 314-320 ◽  
Author(s):  
K. Kuperkar ◽  
A. Patriati ◽  
E.G.R. Putra ◽  
K. Singh ◽  
D.G. Marangoni ◽  
...  
Keyword(s):  
Cetyltrimethylammonium Bromide ◽  
Nuclear Overhauser Effect ◽  
Salt Water ◽  
Total Concentration ◽  
Water System ◽  
2D Nmr ◽  
Spectral Shift ◽  
Micellar Aggregates ◽  
2D Noesy ◽  
Nuclear Overhauser

Interaction of 1-butanol (BuOH) with a cationic surfactant, cetyltrimethylammonium bromide (CTAB) aggregate, in water and salt solution has been studied by viscometry, small-angle neutron scattering (SANS), and 2D-NMR techniques. The experimental results are interpreted in terms of a possible micellar growth occurring in the presence of added alcohol and salt. It was observed that the addition of BuOH strongly influences the viscosity of the CTAB/salt micellar system, reaching a peak viscosity at about 0.5% w/v of BuOH over a range of salt concentrations. Scattering measurements support the idea of a structural transformation by the observation of a spectral shift (broadening) as the total concentration of surfactant varies, indicating a decrease in the intermicellar distance and narrow size distribution. The chemical shift from 1H NMR measurements gave complementary data on the solubilization of BuOH in CTAB micelles, whereas the expected locus (site) of the additive added to the surfactant including the dynamics of the molecules in micellar aggregates were successfully correlated by significant and positive cross peaks obtained from two-dimensional nuclear Overhauser effect spectroscopy (2D-NOESY).

Nuclear Overhauser Effect (NOE) Enhancement of11B NMR Spectra of Borane Adducts in the Solid State

2006 ◽  
Vol 128 (21) ◽  
pp. 6782-6783 ◽  
Author(s):  
Sharon E. Ashbrook ◽  
Nicholas G. Dowell ◽  
Ivan Prokes ◽  
Stephen Wimperis
Keyword(s):  
Solid State ◽  
Nmr Spectra ◽  
Nuclear Overhauser Effect ◽  
Overhauser Effect ◽  
Nuclear Overhauser

The isolation and structural elucidation of a new iridoid glycoside from Cymbaria dahurica L.

2018 ◽  
Vol 73 (6) ◽  
pp. 377-379 ◽  
Author(s):  
Cui-Lan Bai ◽  
Qing-Hu Wang ◽  
Yan-Hua Xu ◽  
Jun-Sheng Han ◽  
Yin-Ping Bao
Keyword(s):  
Quantum Coherence ◽  
Nuclear Overhauser Effect ◽  
Multiple Bond ◽  
2D Nmr ◽  
Iridoid Glycoside ◽  
Correlation Spectroscopy ◽  
Etoac Extract ◽  
Overhauser Effect ◽  
Nuclear Overhauser ◽  
C Nmr

AbstractA new iridoid glycoside, namely, cymdahoside A (1), together with two known ones, 2 and 3, were isolated from the EtOAc extract of Cymbaria dahurica. The structure elucidation of 1 was carried out by one-dimensional (1D) NMR (1H and 13C NMR) and 2D NMR (correlation spectroscopy, heteronuclear single-quantum coherence, heteronuclear multiple-bond correlation and nuclear Overhauser effect spectroscopy) spectral analyses.

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