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21.
Justice AK Linck RC Rauchfuss TB Wilson SR 《Journal of the American Chemical Society》2004,126(41):13214-13215
The photochemical reaction of Ru2(S2C3H6)(CO)4(PCy3)2 (1) and H2 gives the dihydride Ru2(S2C3H6)(mu-H)(H)(CO)3(PCy3)2 (2). NMR and crystallographic studies reveal mutually trans basal phosphine ligands and both bridging and terminal hydrides. Ru2(S2C2H4)(CO)4(PCy3)2 behaves similarly. Other HX substrates undergo photoaddition to 1, affording Ru2(S2C3H6)(mu-H)(X)(CO)3(PCy3)2 for X = OTs (3a), Cl (3b), and SPh (3c). Treatment of Ru2(S2C3H6)(mu-H)(H)(CO)3(PCy3)2 with [H(OEt2)]BArF4 (ArF = B(C6H3-3,5-(CF3)2) in CD2Cl2 gives [Ru2(S2C3H6)(mu-H)(CO)3(PCy3)2(H2)]+ (4), which catalyzes H2-D2 exchange. The reaction of 2 with [D(OEt2)]BArF4 gave [Ru2(S2C3H6)(mu-H)(CO)3(PCy3)2(HD)]+ (JH-D = 31 Hz). These studies provide the first models for the Fe-only hydrogenases that bear dihydrogen and terminal hydrido ligands. 相似文献
22.
J Knapp P Bokník H G Gumbinger B Linck H Lüss F U Müller W Schmitz U Vahlensieck J Neumann 《Journal of chromatographic science》1999,37(5):145-149
A rapid and simple reversed-phase high-performance liquid chromatographic (HPLC) method for the determination of clobazam concentrations in human blood samples is developed and validated. Solid-phase column extraction is performed to clean up blood samples before running the analytical HPLC system. The chromatography is isocratic with a mobile phase consisting of acetonitrile (20%, v/v), methanol (23%, v/v), and 0.1 M potassium hydrogen phosphate buffer (pH 3.6; 57%, v/v) at a constant flow rate of 2 mL/min. Clobazam is detected at 226 nm. Chromatography is completed within less than 25 min. The recovery rate is greater than 95% and linear over a wide range of drug concentrations. The intra-assay coefficient of variation percentage varies between 4.3 and 12. This method is used for therapeutic drug monitoring in patients undergoing antiepileptic therapy with clobazam. Plasma levels of clobazam ranged from 21 to 663 ng/mL. Other antiepileptic compounds, such as clonazepam and phenobarbital, did not interfere with the detection of clobazam. 相似文献
23.
S. Hochberg V. K. La Mer J. Gicklhorn A. Nistler R. Collander N. P. Peskoff A. E. Wright A. Szegvàri Y. P. Liu T. P. Chou H. Y. Fang P. P. T. Sah L. Kofler G. Linck E. Köhler A. E. Sandström Ph. Groß H. Steiner F. Krauss E. A. Hauser C. J. Frosch S. Dushman H. A. Abramson L. S. Moyer A. Voet E. B. Grossman S. Komagata und G. E. van Gils 《Fresenius' Journal of Analytical Chemistry》1939,116(3-4):132-140
Ohne Zusammenfassung 相似文献
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25.
Julio Duque Hctor Novoa de Armas Ramn Poms Hernndez Margarita Surez Navarro Estael Ochoa Rodríguez Esperanza Salfrn Yamila Verdecia Reyes Norbert. M Blaton Oswald M. Peeters Camiel J. De Ranter 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(11):1346-1347
In the title compound, C28H38N4O6, the 4‐aryl substituent occupies a pseudo‐axial position approximately orthogonal to the plane of the dihydropyridine ring [88.1 (3)°]. The dihydropyridine ring adopts a flattened boat conformation. The H atom on the pyridine N atom is involved in a bifurcated intramolecular hydrogen bond, the acceptors being the N atoms of the two piperidylmethyl groups [N?N 2.629 (4) and 2.695 (4) Å]. 相似文献
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27.
de Florian Daniel Fidanza Nerina Hernández-Pinto Roger Mazzitelli Javier Habarnau Yamila Rotstein Sborlini Germán 《The European Physical Journal C - Particles and Fields》2013,73(4):1-5
We analyze a noncommutative model of BTZ spacetime based on deformation of the standard symplectic structure of phase space, i.e., a modification of the standard commutation relations among coordinates and momenta in phase space. We find a BTZ-like solution that is nonperturbative in the non-trivial noncommutative structure. It is shown that the use of deformed commutation relations in the modified non-canonical phase space eliminates the horizons of the standard metric. 相似文献
28.
de Vargas BA Argenta DF Borghetti G Koester LS Bassani VL Teixeira HF 《Journal of chromatographic science》2012,50(2):114-118
Recent studies have shown the effect of soy isoflavones in preventing skin photoaging and photocarcinogenesis, especially for genistein (GEN). Nanoemulsions have been proposed as a delivery system for GEN administration due to the low water solubility of this isoflavone. This article describes the validation of an isocratic liquid chromatography method to determine GEN in porcine ear skin layers from nanoemulsions before and after incorporation into hydrogels. The analyses are performed on a reversed-phase C18 column using a mobile phase composed of methanol-water (70:30, v/v) under acid conditions (at pH 3.0) and UV detection at 270 nm. The method is linear in the range of 0.1-10 μg/mL (r(2) > 0.999) in the presence of skin extracts. The low limit of quantitation is estimated as 0.1 μg/mL. No interferences from formulation excipients or skin layer compounds are detected. The RSD values for intra- and inter-day precision are lower than 15%. Recovery ranged from approximately 90% to 110%. The method is applied to estimate GEN retention in the skin from formulations using Franz diffusion cells. The highest amount of GEN is detected in the epidermis (185 μg/cm(2)). In conclusion, the method proved to be specific, precise, and accurate in determining GEN amounts from formulations in skin retention studies. 相似文献
29.
Margarita Surez Esperanza Salfrn Estael Ochoa Yamila Verdecia Livan Alba Nazario Martín Carlos Seoane Roberto Martínez‐Alvarez Hector Novoa De Armas Norbert M. Blaton Oswald M. Peeters Camiel J. De Ranter 《Journal of heterocyclic chemistry》2003,40(2):269-275
Two dihydropyridines endowed with fluorine atoms ( 3 ) and fluorine and chlorine atoms ( 4 ) have been synthesized and structurally characterized by experimental X‐ray analyses and theoretical calculations at the semiempirical (AMI) and ab initio (HF/6–31G*) levels. The results show that these compounds meet the required criteria to act as potential calcium channel modulators. 相似文献
30.
Mamone G Caira S Garro G Nicolai A Ferranti P Picariello G Malorni A Chianese L Addeo F 《Electrophoresis》2003,24(16):2824-2837
We report a fast and easy-to-use procedure that combines polyacrylamide gel electrophoresis with matrix assisted laser desorption/ionization-time of flight-mass spectrometry (MALDI-TOF) and nanoelectrospray-tandem mass spectrometry (nES-MS/MS) analysis for the identification of casein components and defined phosphorylated sites. This methodology ensured identification of more than 30 phosphorylated proteins, five beta-, fifteen alpha(s1)-, ten alpha(s2)-, and four kappa-casein (CN) components, including nonallelic, differently phosphorylated, and glycosylated forms. The sugar motif covalently bound to kappa-CN was identified as chains, trisaccharide GalNAc, Gal, NeuGc, and tetrasaccharide 1GalNAc, 1Gal, 2NeuGc. Also identified was a biantennary chain made up of both chains of trisaccharide 1GalNAc, 1Gal, 1NeuGc, and tetrasaccharide 1GalNAc, 1Gal, 2NeuGc moiety on a single kappa-CN component. The phosphate group on site Ser12 of tryptic peptide 8-22 of most phosphorylated alpha(s1)-CN (11 phosphate groups) was localized and the oligosaccharide sequence of the main tryptic glycopeptides of two kappa-CN components was determined by means of MS/MS analysis. 相似文献