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Mhamad Aly Moussawi, Nathalie Leclerc-Laronze, Sébastien Floquet, Pavel A Abramov, Maxim Nailyevich Sokolov, Stephane Cordier, Anne Ponchel, Eric Monflier, Herve Bricout, David Landy, Mohamed Haouas, Jerome Marrot, Emmanuel Cadot
Herein, we report on a three-component supramolecular hybrid system built from specific recognition processes involving a Dawson type polyoxometalate [P2W18O62](6-,) a cationic electron-rich cluster {[Ta6Br12(H6O)6]@2CD}(2+) and γ-cyclodextrin. Investigations of such a class of materials have been conducted using bottom-up approach by studying the specific interactions between -CD and both types of inorganic units. Their ability to interact has been investigated in the solid state by single-crystal X-ray diffraction and in solution using multinuclear NMR methods (including DOSY, EXSY and COSY), ESI-mass and UV-vis spectroscopies, electrochemistry and ITC experiments...
August 18, 2017: Journal of the American Chemical Society
F Berride, E Troche-Pesqueira, G Feio, E J Cabrita, T Sierra, A Navarro-Vázquez, M M Cid
Chromonic liquid crystals (CLC) are lyotropic phases formed by discotic mesogens in water. Simple chiral dopants such as amino acids have been reported to turn chromonic liquid crystals into their cholesteric counterparts. Here we report a chirality amplification effect in the nematic phase of a 9 wt% disodium cromoglycate (DSCG) lyotropic liquid crystal (LLC) upon doping with a water-soluble codeine derivative. The transition on cooling the isotropic to the nematic phase showed the presence of homochiral spindle-shaped droplets (tactoids)...
August 18, 2017: Soft Matter
Sharadrao M Patil, David A Keire, Kang Chen
Particle size distribution, a measurable physicochemical quantity, is a critical quality attribute of drug products that needs to be controlled in drug manufacturing. The non-invasive methods of dynamic light scattering (DLS) and Diffusion Ordered SpectroscopY (DOSY) NMR can be used to measure diffusion coefficient and derive the corresponding hydrodynamic radius. However, little is known about their use and sensitivity as analytical tools for particle size measurement of formulated protein therapeutics. Here, DLS and DOSY-NMR methods are shown to be orthogonal and yield identical diffusion coefficient results for a homogenous monomeric protein standard, ribonuclease A...
August 8, 2017: AAPS Journal
Yamina Belabassi, Juliette Moreau, Virginia Gheran, Céline Henoumont, Anthony Robert, Maité Callewaert, Guillaume Rigaux, Cyril Cadiou, Luce Vander Elst, Sophie Laurent, Robert N Muller, Anca Dinischiotu, Sorina Nicoleta Voicu, Francoise Chuburu
To synthesize chitosan nanoparticles (CS NPs), ionic gelation is a very attractive method. It relies on the spontaneous supramolecular assembly of cationic CS with anionic compounds, which leads to nanohydrogels. To extend ionic gelation to functionalized CS, the assessment of CS degree of substitution (DSCS) is a key step. In this paper, we have developed a hyphenated strategy for functionalized CS characterization, based upon 1H, DOSY and when relevant, 1D diffusion-filtered 19F NMR spectroscopies. For that, we have synthesized two series of water-soluble CS via amidation of CS amino groups with mPEG2000-COOH or fluorinated synthons (TFB-COOH)...
August 4, 2017: Biomacromolecules
Saikat Santra, Somnath Bej, Mandira Nandi, Partha Mondal, Pradyut Ghosh
Herein, a bis-amido tris-amine macrocycle and five bipyridine-based bidentate chelating ligands were investigated towards various divalent transition metal ion (Ni(II), Co(II), Cu(II), and Zn(II))-templated syntheses of metallo [2]pseudorotaxanes. The formation of these ternary complexes was elucidated via different spectroscopic techniques such as ESI-MS, absorption spectroscopy, EPR spectroscopy, and single-crystal X-ray diffraction studies wherever possible. Azide-terminated Ni(II), Co(II), Cu(II), Zn(II)-templated [2]pseudorotaxanes were explored to generate [2]rotaxane, ROT, via reaction with an alkyne-terminated triphenylene unit as a stopper under the mild reaction condition of the Cu(I)-catalyzed azide-alkyne cycloaddition reaction...
August 3, 2017: Dalton Transactions: An International Journal of Inorganic Chemistry
Philipp A Elvang, Paul C Stein, Annette Bauer-Brandl, Martin Brandl
No abstract text is available yet for this article.
July 18, 2017: Journal of Pharmaceutical and Biomedical Analysis
Onkei Tai, Russell Hopson, Paul G Williard
Solution characterizations and ligand binding constants were determined for n-butyllithium in hydrocarbon and ethereal solvents using diffusion-ordered NMR. In hydrocarbon solvents, n-butyllithium exists primarily as an octamer at -40 °C and deaggregates to a hexamer when the temperature is increased. In the presence of THF or diethyl ether, n-butyllithium exists predominantly as a tetra-solvated tetramer and deaggregates to a tetra-solvated dimer in the presence of a large excess or neat THF. The ligand binding constants for the tetra-solvated tetramers were measured using (1)H NMR/DOSY titration...
July 27, 2017: Organic Letters
Alexandra Epp, Juliane Hobusch, Yannic C Bartsch, Janina Petry, Gina-Maria Lilienthal, Carolien A M Koeleman, Simon Eschweiler, Christian Möbs, Ashley Hall, Suzanne C Morris, Dominique Braumann, Christine Engellenner, Josephine Bitterling, Johann Rahmöller, Alexei Leliavski, Robina Thurmann, Mattias Collin, Kelley W Moremen, Richard T Strait, Véronique Blanchard, Arnd Petersen, Timo Gemoll, Jens K Habermann, Frank Petersen, Andreas Nandy, Helga Kahlert, Michael Hertl, Manfred Wuhrer, Wolfgang Pfützner, Uta Jappe, Fred D Finkelman, Marc Ehlers
In presence of high allergen dosis besides IgE also IgG antibodies can induce allergic reactions, whose severity is dependent on the induced type of IgG Fc glycosylation, what should be considered for new AIT protocols containing new adjuvants.
July 17, 2017: Journal of Allergy and Clinical Immunology
Alberto Vascellari, Carlo Ramponi, Davide Venturin, Giulia Ben, Davide Blonna, Nicolò Coletti
PURPOSE: The purpose of this study was to evaluate validity and responsiveness of the Degree of Shoulder Involvement in Sport (DOSIS) scale. METHODS: A web-based survey was developed to test the construct validity of the DOSIS scale. Fifty-three patients with a median age of 33 years (range 17-59) were included in the study. Convergent validity was evaluated by external correlation (Spearman's rank correlation coefficient, r) of the DOSIS with the Brophy-Marx and Tegner activity scales, the Western Ontario shoulder instability index (WOSI), the Simple Shoulder Test (SST), and the Short-Form 36 (SF-36)...
July 18, 2017: Knee Surgery, Sports Traumatology, Arthroscopy: Official Journal of the ESSKA
Zhanyao Hou, Wim Dehaen, Joël Lyskawa, Patrice Woisel, Richard Hoogenboom
A novel supramolecular miktoarm star polymer was successfully constructed in water from a pyridine end-decorated polymer (Py-PmDEGA) and a metalloporphyrin based star polymer (ZnTPP-(PEG)4) via metal-ligand coordination. The Py-PmDEGA moiety was prepared via a combination of reversible addition-fragmentation chain transfer polymerization (RAFT) and subsequent aminolysis and Michael addition reactions to introduce the pyridine end-group. The ZnTPP(PEG)4 star-polymer was synthesized by the reaction between tetrakis(p-hydroxyphenyl)porphyrin and toluenesulfonyl-PEG, followed by insertion of a zinc ion into the porphyrin core...
July 25, 2017: Chemical Communications: Chem Comm
Madeleine Piot, Sébastien Hupin, Hélène Lavanant, Carlos Afonso, Laurent Bouteiller, Anna Proust, Guillaume Izzet
The metal-driven self-assembly of a Keggin-based hybrid bearing two remote pyridine units was investigated. The resulting supramolecular species were identified by combination of 2D diffusion NMR spectroscopy (DOSY) and electrospray ionization mass spectrometry (ESI-MS) as a mixture of molecular triangles and squares. This behavior is different from that of the structural analogue Dawson-based hybrid displaying a higher charge, which only led to the formation of molecular triangles. This study highlights the decisive effect of the charge of the POMs in their self-assembly processes that disfavors the formation of large assemblies...
July 17, 2017: Inorganic Chemistry
Shigeto Ueda, Toshiaki Saeki, Akihiko Osaki, Tomohiko Yamane, Ichiei Kuji
Bevacizumab, an antibody against endothelial growth factor, is a key but controversial drug in the treatment of metastatic breast cancer. We, therefore, aimed to determine the intrinsic resistance to bevacizumab at the physiological and molecular levels in advanced breast cancer using positron emission tomography (PET), dynamic contrast-enhanced MRI, diffuse optical spectroscopic imaging (DOSI), and multiplex cytokine assays.<br />Experimental Design: In total, 28 patients diagnosed with stage III/IV advanced breast cancer receiving single-agent bevacizumab for 1 week followed by paclitaxel combined with bevacizumab underwent (18)F-fluorodeoxyglucose (FDG)-PET, (18)F-fluoromisonidazole (FMISO)-PET, and MRI at both baseline and two courses after treatment initiation...
July 5, 2017: Clinical Cancer Research: An Official Journal of the American Association for Cancer Research
Falco Beer, Felix Urbat, Jan Steck, Melanie Huch, Diana Bunzel, Mirko Bunzel, Sabine E Kulling
The heterocyclic aromatic amine (HAA) 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (PhIP) is converted into 7-hydroxy-5-methyl-3-phenyl-6,7,8,9-tetrahydropyrido[3',2':4,5]imidazo[1,2-a]pyrimidin-5-ium chloride (PhIP-M1) via a chemical reaction with 3-hydroxypropionaldehyde or acrolein derived from glycerol by reuterin producing gut bacteria. Because it is unknown whether this reaction also applies to other HAAs, seven foodborne HAAs (2-amino-9H-pyrido[2,3-b]indole (AαC), 3-amino-1,4-dimethyl-5H-pyrido[4,3-b]indole (Trp-P-1), 2-amino-3-methyl-3H-imidazo[4,5-f]quinoline (IQ), 2-amino-3,4-dimethyl-3H-imidazo[4,5-f]quinoline (MeIQ), 2-amino-3,8-dimethyl-3H-imidazo[4,5-f]quinoxaline (MeIQx), 9H-pyrido[3,4-b]indole (norharman), and 1-methyl-9H-pyrido[3,4-b]indole (harman)) were anaerobically incubated with Lactobacillus reuteri DSM 20016 in the presence of glycerol...
August 16, 2017: Journal of Agricultural and Food Chemistry
Sophia Boyoung Strobel, Sylvie Pätzold, Lisa Zimmer, Alexandra Jensen, Alexander Enk, Jessica Cecile Hassel
HINTERGRUND: In der letzten Zeit wurden in der Literatur vermehrt erhöhte Hauttoxizitäten während einer Kombinationstherapie mit BRAF Inhibitoren und Radiotherapie beschrieben. MATERIAL UND METHODIK: Wir berichten über sieben Melanompatienten in einem nicht resezierbaren Stadium III oder IV, die eine kombinierte Behandlung aus Bestrahlung und BRAF-Inhibitor erhielten. ERGEBNISSE: Bei allen Patienten konnte durch die Kombinationstherapie ein gutes lokales Ansprechen erreicht werden...
July 2017: Journal der Deutschen Dermatologischen Gesellschaft, Journal of the German Society of Dermatology: JDDG
Markus M Schreiner, Hannes Platzgummer, Sylvia Unterhumer, Michael Weber, Gabriel Mistelbauer, Christian Loewe, Ruediger E Schernthaner
OBJECTIVES: To investigate radiation exposure, objective image quality, and the diagnostic accuracy of a BMI-adjusted ultra-low-dose CT angiography (CTA) protocol for the assessment of peripheral arterial disease (PAD), with digital subtraction angiography (DSA) as the standard of reference. METHODS: In this prospective, IRB-approved study, 40 PAD patients (30 male, mean age 72 years) underwent CTA on a dual-source CT scanner at 80kV tube voltage. The reference amplitude for tube current modulation was personalized based on the body mass index (BMI) with 120 mAs for [BMI≤25] or 150 mAs for [25<BMI≤30]...
August 2017: European Journal of Radiology
Anniina Kiesilä, Lauri Kivijärvi, Ngong Kodiah Beyeh, Jani Moilanen, Michael Groessl, Filip Topic, Tatiana Rothe, Sven Götz, Kari Rissanen, Arne Lützen, Elina Kalenius
Complex formation between hexafluorophosphate (PF6-) and tetraisobutyl-octahydroxypyridine[4]arene (1) has been thoroughly studied in gas phase (ESI-QTOF-MS, IM-MS, DFT calculations), solid state (X-ray crystallography) and in chloroform solution (1H, 19F and DOSY NMR). In all states of matter, simultaneous endo-complexation of solvent molecules and exo-complexation of PF6- anion within pyridine[4]arene dimer was observed. While similar ternary complex formation is often observed in solid state, this is a unique example of such behaviour in the gas phase that has never been observed so far...
June 30, 2017: Angewandte Chemie
Lucía Cristina Vázquez Cisneros, Patricia López-Uriarte, Antonio López-Espinoza, Mónica Navarro Meza, Ana Cristina Espinoza-Gallardo, Martha Beatriz Guzmán Aburto
La prevalencia e incidencia del sobrepeso y la obesidad continúan en aumento a nivel mundial, así como las enfermedades relacionadas con estas condiciones. Ello se atribuye a un incremento en la ingesta de energía y una disminución en el gasto de la misma. El consumo de té verde se ha relacionado con una reducción en la grasa y el peso corporal. Sin embargo, las investigaciones realizadas con el té verde han sido muy diversas. Esta revisión sistemática explora las investigaciones que se han realizado con té verde y su contenido de galato de epigalocatequina (EGCG) evaluando su efecto sobre la grasa y el peso corporal en humanos...
June 5, 2017: Nutrición Hospitalaria: Organo Oficial de la Sociedad Española de Nutrición Parenteral y Enteral
Maria Julia Ocón Bretón, Ana Isabel Ilundain Gonzalez, Jara Altemir Trallero, Ana Agudo Tabuenca, José Antonio Gimeno Orna
Introducción:la nutrición parenteral total (NPT) es una modalidad de soporte nutricional indicada en aquellas situaciones donde el enfermo no puede cubrir sus requerimientos nutricionales por vía enteral. A pesar de ser una terapia segura y efi caz, no está exenta de complicaciones, entre las que cabe destacar, por su frecuencia, la hipertrigliceridemia. La etiología de esta complicación metabólica es compleja y multifactorial.Objetivos: el objetivo de este trabajo fue determinar los factores de riesgo asociados al desarrollo de hipertrigliceridemia en pacientes adultos hospitalizados no críticos que reciben NPT a corto plazo y evaluar el efecto que una emulsión lipídica enriquecida en ácidos grasos poliinsaturados omega-3 ejerce sobre esta complicación metabólica...
June 5, 2017: Nutrición Hospitalaria: Organo Oficial de la Sociedad Española de Nutrición Parenteral y Enteral
Thomas Swift, Richard Hoskins, Richard Telford, Richard Plenderleith, David Pownall, Stephen Rimmer
Size Exclusion Chromatography is traditionally carried out in either aqueous or non-polar solvents. A system to present molar mass distributions of polymers using methanol as a mobile phase is presented. This is shown to be a suitable system for determining the molar mass distributions poly(N-isopropylacrylamide)s (PNIPAM); a polymer class that is often difficult to analyze by size exclusion chromatography. DOSY NMR was used to provide intrinsic viscosity data that was used in conjunction with a viscometric detector to provide absolute calibration...
July 28, 2017: Journal of Chromatography. A
Lorena M A Silva, Elenilson G Alves Filho, André J Simpson, Marcos R Monteiro, Elaine Cabral, Demian Ifa, Tiago Venâncio
Biodiesel has been introduced as an energetic matrix in several countries around the world. However, the affinity of biodiesel with the components of petrodiesel engines is a growing concern. In order to obtain information regarding the effect of biodiesel on the rubber structure, nuclear magnetic resonance technics under a new technology named as comprehensive multiphase (CMP NMR) and the imaging through desorption electrospray ionization mass spectrometry (DESI-MS imaging) were used. The (1)H CMP-DOSY NMR showed the entrapped fuel into the rubber cavities, which the higher constraint caused by the rubber structure is related to the smaller diffusion coefficient...
October 1, 2017: Talanta
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