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Chenhui Yao, Yang Yang, Shaoan Xu, Haiyan Ma
A series of potassium complexes bearing monoanionic tetradentate amino-phenolate ligands, [LK]2 (L = {(2-R(1))C6H4CH2N[(CH2)2R(2)]CH2(4-R(4)-6-R(3))C6H2O-}, R(1) = NMe2, R(2) = NEt2, R(3) = CPh3, R(4) = Me (1); R(1) = R(2) = NEt2, R(3) = CPh3, R(4) = Me (2); R(1) = NMe2, R(2) = NEt2, R(3) = R(4) = cumyl (4); R(1) = R(2) = OMe, R(3) = (t)Bu, R(4) = Me (6); L = (2-NMe2)C6H4CH2N[[CH2-(S)-1-butylpyrrolidinyl]CH2(4-Me-6-CPh3)C6H2O-] (3)), have been synthesized via reactions of KN(SiMe3)2 and 1 equiv. of the corresponding aminophenols...
April 21, 2017: Dalton Transactions: An International Journal of Inorganic Chemistry
Zhengyu Chen, Brian J Sahli, Mark J MacLachlan
New pyridylsalicylaldimine-based ligands with extended conjugation have been synthesized. The reaction of these ligands with K2PtCl4 yielded triangular Pt3 macrocycles rather than the anticipated Pt4 macrocycles. The macrocycles have been analyzed in solution by variable-temperature and variable-concentration (1)H NMR, NOESY, and DOSY spectroscopy studies. These investigations show that the macrocycles aggregate at room temperature in solution by an entropy-driven process. In the solid state, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry and transmission electron microscopy studies show that the macrocycles aggregate into nanotubular structures...
April 12, 2017: Inorganic Chemistry
Jeffrey Martin Cochran, So Chung, Anaïs Leproux, Wesley Baker, David Busch, Angela DeMichele, Julia Tchou, Bruce Tromberg, Arjun Yodh
We measure tissue blood flow markers in breast tumors during neoadjuvant chemotherapy and investigate their correlation to pathologic complete response in a pilot longitudinal patient study (n=4). Tumor blood flow is quantified optically by diffuse correlation spectroscopy (DCS), and tissue optical properties, blood oxygen saturation, and total hemoglobin concentration are derived from concurrent diffuse optical spectroscopic imaging (DOSI). The study represents the first longitudinal DCS measurement of neoadjuvant chemotherapy in humans over the entire course of treatment; it therefore offers a first correlation between DCS flow indices and pathologic complete response...
April 12, 2017: Physics in Medicine and Biology
Mateusz Dembowski, Christopher A Colla, Sarah Hickam, Anna F Oliveri, Jennifer E S Szymanowski, Allen G Oliver, William H Casey, Peter C Burns
Herein, we report a new salt of a pyrophosphate-functionalized uranyl peroxide nanocluster {U24Pp12} (1) exhibiting Oh molecular symmetry both in the solid and solution. Study of the system yielding 1 across a wide range of pH by single-crystal X-ray diffraction, small-angle X-ray scattering, and a combination of traditional (31)P and diffusion-ordered spectroscopy (DOSY) NMR affords unprecedented insight into the amphoteric chemistry of this uranyl peroxide system. Key results include formation of a rare binary {U24}·{U24Pp12} (3) system observed under alkaline conditions, and evidence of acid-promoted decomposition of {U24Pp12} (1) followed by spatial rearrangement and condensation of {U4} building blocks into the {U32Pp16} (2) cluster...
April 10, 2017: Inorganic Chemistry
Britta Glowacki, Michael Lutter, Hazem Alnasr, Rana Seymen, Wolf Hiller, Klaus Jurkschat
The syntheses of the novel amino alcohols NH(CH2CMe2OH)2(CMe2CH2OH) (1) and N(CH2CMe2OH)(CMe2CH2OH)(CH2CH2OH) (2) as well as the stannatranes N(CH2CMe2O)(CMe2CH2O)(CH2CH2O)SnX (3, X = Ot-Bu), N(CH2CMe2O)3SnOC(O)C9H13O2, 4, and germatranes N(CH2CMe2O)(CMe2CH2O)(CH2CH2O)GeX (5, X = OEt; 6, X = Br) are reported. The compounds were characterized by (1)H, (13)C (1-6), (119)Sn (3, 4), and (15)N (2, 3, 5) NMR and IR spectroscopy, electrospray ionization mass spectrometry, and single crystal X-ray diffraction analysis...
April 10, 2017: Inorganic Chemistry
Bo Song, Zhe Zhang, Kun Wang, Chih-Hao Hsu, Olapeju Bolarinwa, Jing Wang, Yiming Li, Guang-Qiang Yin, Edwin Rivera, Hai-Bo Yang, Changlin Liu, Bingqian Xu, Xiaopeng Li
Two- and three-dimensional metallosupramolecules shaped like a Star of David were synthesized by the self-assembly of a tetratopic pyridyl ligand with a 180° diplatinum(II) motif and Pd(II) ions, respectively. In contrast to other strategies, such as template-directed synthesis and stepwise self-assembly, this design enables the formation of 2D and 3D structures in one step and high yield. The structures were characterized by both one-dimensional ((1) H, (13) C, (31) P) and two-dimensional (COSY, NOESY, DOSY) NMR spectroscopy, ESI-MS, ion-mobility mass spectrometry (IM-MS), AFM, and TEM...
April 6, 2017: Angewandte Chemie
Paul McKeown, James Brown-Humes, Matthew G Davidson, Mary F Mahon, Timothy J Woodman, Matthew D Jones
A range of ligands based upon 2-(aminomethyl)piperidine have been successfully complexed to Mg(ii), Zn(ii) and group IV metal centres. These complexes have been characterised both in solution and solid state with different coordination geometries realised dependant on the nature of the ligand. For the Mg(ii) and Zn(ii) complexes, M(1-2)2, were isolated and analysed by DOSY NMR spectroscopy. These ligands also furnished diastereomeric group IV complexes, M(1-2)2(O(i)Pr)2. Group IV salalen and salan complexes, M(4-5)(OR)2 were also found to be diastereomeric in nature, with either β-cis or α-cis geometriesrespectively...
April 11, 2017: Dalton Transactions: An International Journal of Inorganic Chemistry
Manas Jana, Anirban Ghosh, Abhishek Santra, Rajiv Kumar Kar, Anup Kumar Misra, Anirban Bhunia
HYPOTHESIS: The interaction of lysozyme with the N-acetylmuramic acid (NAM) and N-acetylglucosamine (NAG) unit of peptidoglycan (PGN) polymer of the bacterial cell wall is of immense importance to understand the mechanism of lysozyme on PGN. EXPERIMENTS: The synthesis of three novel NAM derivatives containing fused oxazinone ring to the NAM moiety has been achieved. The synthesized compounds were evaluated for their potential as a glycomimetic acceptor of lysozyme using different biophysical and computational methods such as (1)H NMR, STD NMR, DOSY and Molecular docking...
March 16, 2017: Journal of Colloid and Interface Science
Bin Yuan, Yiming Ding, Ghulam M Kamal, Limin Shao, Zhiming Zhou, Bin Jiang, Peng Sun, Xu Zhang, Maili Liu
2D diffusion-ordered NMR spectroscopy (DOSY) has been widely recognized as a powerful tool for analyzing mixtures and probing inter-molecular interactions in situ. But it is difficult to differentiate molecules with similar diffusion coefficients in presence of overlapped spectra. Its performance is susceptible to the number of chemical components, and usually gets worse when the number of components increases. Here, to alleviate the problem, numerical simultaneous inversion of Laplace transform (SILT) of many related variables is proposed for reconstructing DOSY spectrum (SILT-DOSY)...
March 7, 2017: Journal of Magnetic Resonance
Ziang Li, Lindsay M Johnson, Ralm G Ricarte, Letitia J Yao, Marc A Hillmyer, Frank S Bates, Timothy P Lodge
Blends of hydroxypropyl methylcellulose acetate succinate (HPMCAS) and dodecyl (C12)-tailed poly(N-isopropylacrylamide) (PNIPAm) were systematically explored as a model system to dispense the active ingredient phenytoin by rapid dissolution, followed by the suppression of drug crystallization for an extended period. Dynamic and static light scattering revealed that C12-PNIPAm polymers, synthesized by reversible addition-fragmentation chain-transfer polymerization, self-assembled into micelles with dodecyl cores in phosphate-buffered saline (PBS, pH 6...
March 10, 2017: Langmuir: the ACS Journal of Surfaces and Colloids
Simon Dulz, Niels H Asselborn, Klaus-Peter Dieckmann, Cord Matthies, Walter Wagner, Jens Weidmann, Christoph Seidel, Christoph Oing, Lars A Berger, Winfried Alsdorf, Blanche Mankichian, Christian Meyer, Malte W Vetterlein, Philipp Gild, Tim A Ludwig, Armin Soave, Philipp Schriefer, Andreas Becker, Sascha A Ahyai, Karin Oechsle, Carsten Bokemeyer, Lars Wagenfeld, Margit Fisch, Michael Hartmann, Felix K-H Chun, Luis A Kluth
PURPOSE: Visual impairment represents an infrequent form of cisplatin-induced neurotoxicity; however, visual deterioration has been reported in several studies. To evaluate potential morphological and functional retinal alterations in patients with germ cell cancer (GCC) treated with cisplatin-based chemotherapy (CBC). METHODS: Multi-disciplinary and multi-institutional study design. Examination of 28 eyes of 14 male GCC patients, who had received at least one cycle of CBC...
March 9, 2017: Journal of Cancer Research and Clinical Oncology
Jae Min Choi, Kyeonghui Park, Benel Lee, Daham Jeong, Someshwar D Dindulkar, Youngjin Choi, Eunae Cho, Seyeon Park, Jae-Hyuk Yu, Seunho Jung
Ciprofloxacin is a broad-spectrum fluoroquinolone antibiotic used to treat bacterial infections; however, its limited aqueous solubility inhibits its broader clinical uses. This study investigated the complexation effect of mono-6-deoxy-6-aminoethylamino-β-cyclodextrin on the aqueous solubility and bioavailability of ciprofloxacin. During complexation, the oval-shaped cavity induced by mono-aminoethylamine substitution on the primary rim of β-cyclodextrin, was considered to be a key factor according to NMR spectroscopy and molecular modeling studies...
May 1, 2017: Carbohydrate Polymers
Stefano Parodi, Corrado Dosi, Antonella Zambon, Enrico Ferrari, Marco Muselli
Identifying potential risk factors for problem gambling (PG) is of primary importance for planning preventive and therapeutic interventions. We illustrate a new approach based on the combination of standard logistic regression and an innovative method of supervised data mining (Logic Learning Machine or LLM). Data were taken from a pilot cross-sectional study to identify subjects with PG behaviour, assessed by two internationally validated scales (SOGS and Lie/Bet). Information was obtained from 251 gamblers recruited in six betting establishments...
March 2, 2017: Journal of Gambling Studies
Artur Kasprzak, Magdalena Poplawska, Hanna Krawczyk, Sergey Molchanov, Mikolaj Kozlowski, Michal Bystrzejewski
ABSTRACT: The synthesis of a novel supramolecular system comprising of branched polyethylenimine and cyclodextrin, is presented. The synthesis route is based on the self-assembly phenomena with the inclusion of solvent molecules. The systems are formed by a hydrogen-bonding network and host-guest type interactions between the building blocks. It was found that the native cyclodextrin and polyethylenimine are able to form stable systems when the reaction medium constitutes a polar solvent forming host-guest type complexes with cyclodextrin...
2017: Journal of Inclusion Phenomena and Macrocyclic Chemistry
Leo Richter, Igor Vujic, Alma Sesti, Babak Monshi, Martina Sanlorenzo, Christian Posch, Klemens Rappersberger
HINTERGRUND UND ZIELE: Biologika werden häufig zur Behandlung der Psoriasis eingesetzt und wurden in zahlreichen klinischen Studien getestet. Allerdings können sich Wirkungen und Nebenwirkungen (AEs) bei "real-world"-Patienten unterscheiden, da diese keiner solch strengen Auswahl und Überwachung unterzogen werden. Wir haben Therapieadhärenz ("Medikamenten-Überlebenszeit"), Wirksamkeit und AEs (Qualität, Zeitpunkt des Auftretens) bei "real-world"-Psoriasis-Patienten, die mit Etanercept, Adalimumab oder Ustekinumab behandelt wurden, untersucht...
March 2017: Journal der Deutschen Dermatologischen Gesellschaft, Journal of the German Society of Dermatology: JDDG
Virginia Santesteban Moriones, Javier Ibáñez Santos
Introducción: muy pocos suplementos nutricionales han demostrado científicamente su eficacia como ayuda ergogénica. Esta revisión analizará el monohidrato de creatina (MC), el β-hidroxi-β-metilbutirato (HMB), el bicarbonato sódico (BS), la β-alanina y la cafeína.Objetivos: analizar la eficacia, mecanismos de acción, dosis, efectos adversos y algunos deportes que se pueden beneficiar de su consumo.Métodos: búsqueda en la base de datos PubMed de revisiones bibliográficas de los últimos 15 años y artículos originales de los últimos 5 años de las sustancias estudiadas...
February 1, 2017: Nutrición Hospitalaria: Organo Oficial de la Sociedad Española de Nutrición Parenteral y Enteral
Gábor Orgován, Imre Gonda, Béla Noszál
Biorelevant, isomer-specific physicochemical parameters of resveratrol, a multifunctional component in red wines, with cardioprotective, anti-Alzheimer and several other pharmacologic activities were determined. The parameters include site-specific basicities, lipophilicities, solubilities and diffusion constants for the two geometric isomers. The protonation equilibria of (E)- and (Z)-resveratrol were monitored by (1)H NMR-pH titrations. Five closely related auxiliary compounds ((E)-pinostilbene, (Z)-pinostilbene, (E)-pterostilbene, (Z)-pterostilbene and resorcinol) were also studied...
December 19, 2016: Journal of Pharmaceutical and Biomedical Analysis
Leandro Araújo de Azevedo, Leonis Lourenço da Luz, Jamylle Nunes de Souza Ferro, Emiliano Barreto, Ricardo Oliveira Silva, Severino Alves, Iane Bezerra Vasconcelos Alves
The supramolecular nano-aggregate CUR-CB[7] (CUR = curcumin and CB[7] = cucurbit[7]uril) was efficiently prepared by mixing CUR and CB[7] at a molar ratio of 1 : 1 in ethanol at room temperature. The supramolecular aggregate formation was evidenced by mainly FTIR, (1)H NMR, DOSY and spectroscopy experiments. The supramolecular arrangement promotes the increase in the solubility and stability of CUR without affecting the biological properties of the A549 cells. The luminescence properties of CUR and CUR-CB[7] show anti-Kasha's rule fluorescence, and their remarkable NIR emission enables this material to be used as a luminescent probe and marker for in vivo tracking and structural integrity monitoring of the supramolecular complex...
February 22, 2017: Photochemical & Photobiological Sciences
Ioannis Dosis, Marina Ricci, Laszlo Majoros, Roberto Lava, Håkan Emteborg, Andrea Held, Hendrik Emons
In the context of supporting the EU Member States in the implementation of the EU Water Framework Directive (WFD), a project for the production of a fish reference material (ERM-CE100) certified for its content of the two priority substances hexachlorobenzene (HCB) and hexachlorobutadiene (HCBD) was carried out at the Joint Research Centre (JRC) of the European Commission. The starting material was naturally contaminated Wels catfish (Silurus glanis), caught in the Ebro River (Spain). A novel approach for the processing of the fish was tested that resulted in a homogeneous and stable reference material in the form of a wet paste...
February 21, 2017: Analytical Chemistry
Indrek Reile, Ruud L E G Aspers, Martin C Feiters, Floris P J T Rutjes, Marco Tessari
DOSY analysis can resolve analytes according to their molecular size, offering a complementary way to traditional 2D NMR spectroscopy in the study of chemical mixtures. Applications are, however, limited if analytes have similar shape and size, as is the case in isomer mixtures. Herein we show how solvent effects in methanol-d4 , a common solvent in NMR laboratories, allow to overcome this limitation and provide increased separation of isomeric compounds. Clear NMR signal separation of eight structurally related analytes within a molecular weight (MW) range of three units is demonstrated, allowing unambiguous analysis of a mixture that would have otherwise been unsuitable for DOSY...
February 20, 2017: Magnetic Resonance in Chemistry: MRC
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