Search results for " nuclear magnetic resonance spectroscopy"
showing 10 items of 173 documents
Two-dimensional nuclear magnetic resonance spectroscopy with a microfluidic diamond quantum sensor
2019
Quantum sensors based on nitrogen-vacancy centers in diamond have emerged as a promising detection modality for nuclear magnetic resonance (NMR) spectroscopy owing to their micron-scale detection volume and non-inductive based detection. A remaining challenge is to realize sufficiently high spectral resolution and concentration sensitivity for multidimensional NMR analysis of picoliter sample volumes. Here, we address this challenge by spatially separating the polarization and detection phases of the experiment in a microfluidic platform. We realize a spectral resolution of 0.65 +/- 0.05 Hz, an order-of-magnitude improvement over previous diamond NMR studies. We use the platform to perform …
Hyperbranched poly(glycolide) copolymers with glycerol branching points via ring-opening copolymerization
2015
Abstract Sn(Oct) 2 -catalyzed synthesis of hyperbranched poly(glycolide) copolymers with glycerol branching points in the backbone is possible via ring-opening multi-branching copolymerization (ROMBP) of glycolide and 5HDON (5-hydroxymethyl-1,4-dioxan-2-one). Using this strategy, well-defined and soluble branched polyesters with apparent molecular weights (M n ) in the range of 1300–2000 g mol −1 and varying comonomer content (5HDON/glycolide = 30:70–70:30) were obtained. 2D NMR spectroscopy, thermal analysis and MALDI-TOF mass spectrometry confirmed the successful incorporation of both monomers and the resulting branched structure. Multiple end group functionality offers the possibility fo…
Conformational Changes and Charge Transfer in Biomolecules Resolved Using Dynamic Enhanced Raman Correlation Spectroscopy
2019
International audience; In this contribution, we report that conforma-tional changes of molecules that are often buried in a wide-distributed Gaussian distribution can be discerned by analyzing the dynamics of specific Raman lines. We investigate the pertinence of the auto-and cross-correlation functions applied to the dynamics of three Raman lines of an amino acid, the tryptophan. The cross-correlation between intensity and the Raman band is an indicator of the charge transfer during the diffusion limited reaction of tryptophan and the gold surface. The Pećlet number Pe can provide a valuable indicator of the convective and/or diffusive features of each Raman band. Adsorption induced confo…
Chemical constituents from leaves and root bark of Trichilia monadelpha (Meliaceae)
2018
Abstract Two new limonoid derivatives designated, monadelphin A (1) and monadelphin B (2) and two new sesquiterpene derivatives named trichins A (3) and B (4) were isolated together with six known compounds (5–10) from the mixture of methylene chloride/methanol (1:1) extract of leaves and root bark of Trichilia monadelpha (Meliaceae) collected in Cameroon. The structures of the new compounds were unambiguously established by detailed spectroscopic analysis including 1D and 2D NMR data in conjunction with high resolution mass spectrometry data and by comparison of these data with those of related compounds described in the literature. Compounds 1–4 were screened for their cytotoxic potential…
Hederagenin glycosides from the fruits of Blighia unijugata
2019
Abstract A phytochemical investigation of Blighia unijugata led to the isolation of eleven hederagenin glycosides. Among these compounds, six are previously undescribed, two are described in their native forms for the first time and three are known whereas firstly isolated from Blighia unijugata. The structure of the undescribed compounds was elucidated on the basis of 2D NMR and mass spectrometry analyses as 3-O-β-D-xylopyranosyl-(1 → 3)-α-L-arabinopyranosyl-(1 → 4)-β-D-glucopyranosyl-(1 → 3)-α-L-rhamnopyranosyl-(1 → 2)-α-L-arabinopyranosylhederagenin, 3-O-β-D-xylopyranosyl-(1 → 3)-α-L-arabinopyranosyl-(1 → 4)-3-O-acetyl-β-D-glucopyranosyl-(1 → 3)-α-L-rhamnopyranosyl-(1 → 2)-α-L-arabinopyr…
Nuclear magnetic resonance spectroscopic study of beta-lactoglobulin interactions with two flavor compounds, gamma-decalactone and beta-ionone.
2002
Interactions between a well-characterized protein, beta-lactoglobulin, and two flavor compounds, beta-ionone and gamma-decalactone, were studied by 2D NMR spectroscopy. NMR spectra were recorded in aqueous solution (pH 2.0, 12 mM NaCl, 10% D(2)O) under conditions such that beta-lactoglobulin is present in a monomeric state. TOCSY and NOESY spectra were recorded on the protein and the complexes between protein and ligands. The spectra of the NH-CH(alpha) region showed the cross-signals due to the coupling between N- and C-bonded protons in the polypeptide backbone. The observed chemical shift variations in the presence of ligands can be assigned to changes in the protein conformation. It app…
High-resolution solution NMR structure of the Z domain of staphylococcal protein A
1997
Staphylococcal protein A (SpA) is a cell-wall-bound pathogenicity factor from the bacterium Staphylococcus aureus. Because of their small size and immunoglobulin (IgG)-binding activities, domains of protein A are targets for protein engineering efforts and for the development of computational approaches for de novo protein folding. The NMR solution structure of an engineered IgG-binding domain of SpA, the Z domain (an analog of the B domain of SpA), has been determined by simulated annealing with restrained molecular dynamics on the basis of 671 conformational constraints. The Z domain contains three well-defined alpha-helices corresponding to polypeptide segments Lys7 to Leu17 (helix 1), G…
Polyketide Derivatives from Mangrove Derived Endophytic Fungus Pseudopestalotiopsis theae
2020
Chemical investigation of secondary metabolites from the endophytic fungus Pseudopestalotiopsis theae led to the isolation of eighteen new polyketide derivatives, pestalotheols I&ndash
The unique structure of complete lipopolysaccharide isolated from semi-rough Plesiomonas shigelloides O37 (strain CNCTC 39/89) containing (2S)-O-(4-o…
2013
The complete structure of semi-rough lipopolysaccharide (SR-LPS) of Plesiomonas shigelloides CNCTC 39/89 (serotype O37) has been investigated by (1)H and (13)C NMR spectroscopy, matrix-assisted laser-desorption/ionization time-of-flight MS, and chemical methods. The following structure of the single unit of the O-antigen has been established: [formula see text] in which α-D-Lenp is (2S)-O-(4-oxopentanoic acid)-α-D-Glcp residue which has not been found in nature. The absolute configuration of oxopentanoic acid moiety in α-d-Lenose residue was determined by NOESY experiment combined with molecular modeling (MM2 force field). The decasaccharide core is substituted at C-4 of the β-D-Glcp residu…
Detecting ni(ii) in aqueous solution by 3-(2-pyridyl)-[1,2,3]triazolo[1,5-a]pyridine and dimethyl-beta-cyclodextrin
2013
Abstract A new supramolecular sensitizer for nickel(II) ion in aqueous solution based on a pyridyltriazolopyridine-cyclodextrin inclusion complex is proposed. The inclusion complexation behavior, characterization and binding ability of pyridyltriazolopyridine (PTP) with dimethyl-β-cyclodextrin (DMβCD) has been investigated both in solution and solid state by means of absorption, fluorescence, 1H NMR, DSC, and molecular modeling methods. The stoichiometry of the inclusion complex is 1:1, and the thermodynamic studies indicate that the inclusion of PTP is mainly an entropic driven process. The 2D NMR studies revealed that the pyridyl-triazolopyridine is included by both sides of cyclodextrin …