Search results for " nuclear magnetic resonance"
showing 10 items of 248 documents
Equipping metallo-supramolecular macrocycles with functional groups: Assemblies of pyridine-substituted urea ligands
2012
A series of di-(m-pyridyl)-urea ligands were prepared and characterized with respect to their conformations by NOESY experiments and crystallography. Methyl substitution in different positions of the pyridine rings provides control over the position of the pyridine N atoms relative to the urea carbonyl group. The ligands were used to self-assemble metallo-supramolecular M(2)L(2) and M(3)L(3) macrocycles which are generated in a finely balanced equilibrium in DMSO and DMF according to DOSY NMR experiments and ESI FTICR mass spectrometry. Again, crystallography was used to characterize the assemblies. Methyl substitution in positions next to the pyridine nitrogen prevents coordination, while …
New Acyclic Cytotoxic Jasplakinolide Derivative from the Marine Sponge Jaspis splendens
2019
A new acylic jasplakinolide congener (2), another acyclic derivative requiring revision (4), together with two jasplakinolide derivatives including the parent compound jasplakinolide (1) were isolated from the Indonesian marine sponge Jaspis splendens. The chemical structures of the new and known compounds were unambiguously elucidated based on HRESIMS and exhaustive 1D and 2D NMR spectral analysis as well as a comparison of their NMR data with those of jasplakinolide (1). The isolated jasplakinolides inhibited the growth of mouse lymphoma (L5178Y) cells in vitro with IC50 values in the low micromolar to nanomolar range.
2021
Centaurothamnus maximus (family Asteraceae), is a leafy shrub indigenous to the southwestern Arabian Peninsula. With a paucity of phytochemical data on this species, we set out to chemically characterize the plant. From the aerial parts, two newly identified guaianolides were isolated: 3β-hydroxy-4α(acetoxy)-4β(hydroxymethyl)-8α-(4-hydroxy methacrylate)-1αH,5αH, 6αH-gual-10(14),11(13)-dien-6,12-olide (1) and 15-descarboxy picrolide A (2). Seven previously reported compounds were also isolated: 3β, 4α, 8α-trihydroxy-4-(hydroxymethyl)-lαH, 5αH, 6βH, 7αH-guai-10(14),11(13)-dien-6,12-olide (3), chlorohyssopifolin B (4), cynaropikrin (5), hydroxyjanerin (6), chlorojanerin (7), isorhamnetin (8), …
Triterpene saponins of the root bark of Olax obtusifolia De Wild
2018
Abstract Four undescribed triterpenoid saponins together with five known and oleanolic acid were isolated from root bark of Olax obtusifolia De Wild. Their structures were elucidated by spectroscopic methods including 1D and 2D NMR experiments, in combination with mass spectrometry as 3-O-α- l -rhamnopyranosyl-(1→4)-α- l -rhamnopyranosyl-(1→3)-β- d -glucuronopyranosyloleanolic acid, 3-O-α- l -rhamnopyranosyl-(1→4)-α- l -rhamnopyranosyl-(1→3)-β- d -glucuronopyranosyloleanolic acid 28-O-β- d -glucopyranosyl ester, 3-O-α- l -rhamnopyranosyl-(1→3)-β- d -glucopyranosyl-(1→2)-[β- d -glucopyranosyl-(1→3)]-β- d -glucuronopyranosyloleanolic acid and 3-O-α- l -rhamnopyranosyl-(1→3)-β- d -glucopyranos…
Adsorption equilibria of water vapor on cork.
2010
International audience; We report here for the first time a complete thermodynamic study of water vapor adsorption on crude cork powder and plate. Adsorption−desorption isotherms were accurately measured by thermogravimetry at 283, 298, and 313 K in a large range of relative pressure. Adsorption enthalpies were determined by calorimetry as a function of loading. Adsorption−desorption isotherms exhibit a hysteresis due to the swelling of the material. The influence of the presence of lenticels on the adsorption properties of cork is found to be negligible. A detailed analysis and interpretation of adsorption data allow proposal of an adsorption mechanism in two steps. (i) First, water adsorb…
27Al NMR Study of the pH Dependent Hydrolysis Products of Al2(SO4)3 in Different Physiological Media
2018
Soluble inorganic aluminium compounds like aluminium sulfate or aluminium chloride have been challenged by the European Chemical Agency to induce germ cell mutagenicity. Before conducting mutagenicity tests, the hydrolysis products in water and in physiological solutions should be determined as a function of the concentration and pH. We used different 27Al NMR spectroscopic techniques (heteronuclear Overhauser effect spectroscopy (HOESY), exchange spectroscopy (EXSY), diffusion ordered (DOSY)) in this work to gain the information to study the aluminium species in solutions with Al2(SO4)3 concentrations of 50.0, 5.0, and 0.5 g/L and their pH and time dependent transformation. At low pH, thre…
Structural characterization of polysaccharides of a productive strain of the culinary-medicinal king oyster mushroom, pleurotus eryngii (Agaricomycet…
2018
A preliminary biological investigation of the dry basidiomata of strain C-142-c of Pleurotus eryngii has shown significant antioxidant activity. Two different polysaccharides (PEPS-A1 and PEPS-A2) were isolated from the cultivated edible mushroom, P. eryngii C-142-c strain. Based on acid hydrolysis, methylation analysis, and nuclear magnetic resonance experiments (1H, 13C, distortionless enhancement by polarization transfer, double quantum filtered correlation spectroscopy, total correlation spectroscopy, nuclear Overhauser effect spectroscopy, heteronuclear singlequantum correlation spectroscopy, and heteronuclear multiple-bond correlation spectroscopy), the structures of the repeating uni…
The cytoprotective protein MANF promotes neuronal survival independently from its role as a GRP78 cofactor
2021
Mesencephalic astrocyte-derived neurotrophic factor (MANF) is an endoplasmic reticulum (ER)-stress-regulated protein exhibiting cytoprotective properties through a poorly understood mechanism in various in vitro and in vivo models of neuronal and non-neuronal damage. Although initially characterized as a secreted neurotrophic factor for midbrain dopamine neurons, MANF has recently gained more interest for its intracellular role in regulating the ER homeostasis, including serving as a cofactor of the chaperone glucose-regulated protein 78 (GRP78). We aimed for a better understanding of the neuroprotective mechanisms of MANF. Here we show for the first time that MANF promotes the survival of …
Urinary Metabolic Signatures Detect Recurrences in Non-Muscle Invasive Bladder Cancer
2019
Patients with non-muscle invasive bladder cancer (NMIBC) undergo lifelong monitoring based on repeated cystoscopy and urinary cytology due to the high recurrence rate of this tumor. Nevertheless, these techniques have some drawbacks, namely, low accuracy in detection of low-grade tumors, omission of pre-neoplastic lesions and carcinomas in situ (CIS), invasiveness, and high costs. This work aims to identify a urinary metabolomic signature of recurrence by proton Nuclear Magnetic Resonance (1H NMR) spectroscopy for the follow-up of NMIBC patients. To do this, changes in the urinary metabolome before and after transurethral resection (TUR) of tumors are analyzed and a Partial Least Square Dis…
A community resource of experimental data for NMR / X-ray crystal structure pairs
2015
We have developed an online NMR / X-ray Structure Pair Data Repository. The NIGMS Protein Structure Initiative (PSI) has provided many valuable reagents, 3D structures, and technologies for structural biology. The Northeast Structural Genomics Consortium was one of several PSI centers. NESG used both X-ray crystallography and NMR spectroscopy for protein structure determination. A key goal of the PSI was to provide experimental structures for at least one representative of each of hundreds of targeted protein domain families. In some cases, structures for identical (or nearly identical) constructs were determined by both NMR and X-ray crystallography. NMR spectroscopy and X-ray diffraction …