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Matthias Brendel Carolin Braun Dr. Frank Rominger Prof. Dr. Peter Hofmann 《Angewandte Chemie (International ed. in English)》2014,53(33):8741-8745
For a long time d10‐ML2 fragments have been known for their potential to activate unreactive bonds by oxidative addition. In the development of more active species, two approaches have proven successful: the use of strong σ‐donating ligands leading to electron‐rich metal centers and the employment of chelating ligands resulting in a bent coordination geometry. Combining these two strategies, we synthesized bis‐NHC chelate complexes of nickel(0) and platinum(0). Bis(1,5‐cyclooctadiene)nickel(0) and ‐platinum(0) react with bisimidazolium salts, deprotonated in situ at room temperature, to yield tetrahedral or trigonal‐planar bis‐NHC chelate olefin complexes. The synthesis and characterization of these complexes as well as a first example of C? C bond activation with these systems are reported. Due to the enforced cis arrangement of two NHCs, these compounds should open interesting perspectives for bond‐activation chemistry and catalysis. 相似文献
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Copper(I)‐Catalyzed Regioselective Addition of Nucleophilic Silicon Across Terminal and Internal Carbon–Carbon Triple Bonds 下载免费PDF全文
The copper(I) alkoxide‐catalyzed release of a silicon‐based cuprate reagent from a silicon–boron pronucleophile is applied to the addition across carbon–carbon triple bonds. Commercially available CuBr?Me2S was found to be a general precatalyst that secures high regiocontrol for both aryl‐ and alkyl‐substituted terminal as well as internal alkynes. The solvent greatly influences the regioisomeric ratio, favoring the linear regioisomer with terminal acceptors. This facile protocol even allows for the transformation of internal acceptors with remarkable levels of regio‐ and diastereocontrol. 相似文献
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Christian Wenz Coral Barbas Ángeles López‐Gonzálvez Antonia Garcia Fernando Benavente Victoria Sanz‐Nebot Tim Blanc Gordon Freckleton Philip Britz‐McKibbin Meera Shanmuganathan Francois de l′Escaille Johann Far Rob Haselberg Sean Huang Carolin Huhn Martin Pattky David Michels Si Mou Feng Yang Christian Neusuess Nora Tromsdorf Edward E.K. Baidoo Jay D. Keasling SungAe Suhr Park 《Journal of separation science》2015,38(18):NA-NA
A collaborative study on the robustness and portability of a capillary electrophoresis‐mass spectrometry method for peptide mapping was performed by an international team, consisting of 13 independent laboratories from academia and industry. All participants used the same batch of samples, reagents and coated capillaries to run their assays, whereas they utilized the capillary electrophoresis‐mass spectrometry equipment available in their laboratories. The equipment used varied in model, type and instrument manufacturer. Furthermore, different types of sheath‐flow capillary electrophoresis–mass spectrometry interfaces were used. Migration time, peak height and peak area of ten representative target peptides of trypsin‐digested bovine serum albumin were determined by every laboratory on two consecutive days. The data were critically evaluated to identify outliers and final values for means, repeatability (precision within a laboratory) and reproducibility (precision between laboratories) were established. For relative migration time the repeatability was between 0.05 and 0.18% RSD and the reproducibility between 0.14 and 1.3% RSD. For relative peak area repeatability and reproducibility values obtained were 3–12 and 9–29% RSD, respectively. These results demonstrate that capillary electrophoresis‐mass spectrometry is robust enough to allow a method transfer across multiple laboratories and should promote a more widespread use of peptide mapping and other capillary electrophoresis‐mass spectrometry applications in biopharmaceutical analysis and related fields. 相似文献
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Stilbenes and zeranol are nonsteroidal estrogenic growth promoters which are banned in the European Union (EU) for use in
food-producing animals by Council Directive 96/22/EC. A liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was
developed for the screening and confirmation of stilbenes (diethylstilbestrol, dienestrol, hexestrol) and resorcylic acid
lactones (zeranol and its metabolites taleranol and zearalanone as well as the mycotoxins α-zearalenol, β-zearalenol and zearalenone)
in bovine urine. The method permits the confirmation and quantification of stilbenes and resorcylic acid lactones at levels
below 1 μg L−1 and 1.5 μg L−1, respectively. The validation was carried out according to Commission Decision 2002/657/EC, Chap. 3.1.3 “alternative validation”
by a matrix-comprehensive in-house validation concept. Decision limit CCα, detection capability CCβ, recovery, repeatabiliy,
within-laboratory reproducibility and the uncertainty of measurement were calculated. Furthermore, a factorial effect analysis
was carried out to identify factors that have a significant influence on the method. Factors considered to be relevant for
the method in routine analysis (e.g. operator, matrix condition, storage duration of the extracts before measurement, different
cartridge lots, hydrolysis conditions) were systematically varied on two levels. The factorial analysis showed that different
cartridge lots, storage durations and matrix conditions can exert a relevant influence on the method. 相似文献
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Holland JT Lau C Brozik S Atanassov P Banta S 《Journal of the American Chemical Society》2011,133(48):19262-19265
Optimizing the electrical communication between enzymes and electrodes is critical in the development of biosensors, enzymatic biofuel cells, and other bioelectrocatalytic applications. One approach to address this limitation is the attachment of redox mediators or relays to the enzymes. Here we report a simple genetic modification of a glucose oxidase enzyme to display a free thiol group near its active site. This facilitates the site-specific attachment of a maleimide-modified gold nanoparticle to the enzyme, which enables direct electrical communication between the conjugated enzyme and an electrode. Glucose oxidase is of particular interest in biofuel cell and biosensor applications, and the approach of "prewiring" enzyme conjugates in a site-specific manner will be valuable in the continued development of these systems. 相似文献
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The presented multi-method was developed for the confirmation of 37 antibiotic substances from the six antibiotic groups: macrolides, lincosamides, quinolones, tetracyclines, pleuromutilines and diamino-pyrimidine derivatives. All substances were analysed simultaneously in a single analytical run with the same procedure, including an extraction with buffer, a clean-up by solid-phase extraction, and the measurement by liquid chromatography tandem mass spectrometry in ESI+ mode. The method was validated on the basis of an in-house validation concept with factorial design by combination of seven factors to check the robustness in a concentration range of 5-50 μg kg(-1). The honeys used were of different types with regard to colour and origin. The values calculated for the validation parameters-decision limit CCα (range, 7.5-12.9 μg kg(-1)), detection capability CCβ (range, 9.4-19.9 μg kg(-1)), within-laboratory reproducibility RSD(wR) (<20% except for tulathromycin with 23.5% and tylvalosin with 21.4 %), repeatability RSD(r) (<20% except for tylvalosin with 21.1%), and recovery (range, 92-106%)-were acceptable and in agreement with the criteria of Commission Decision 2002/657/EC. The validation results showed that the method was applicable for the residue analysis of antibiotics in honey to substances with and without recommended concentrations, although some changes had been tested during validation to determine the robustness of the method. 相似文献
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Christian P. Klaus Carolin Thiemann Jürgen Kopf Paul Margaretha 《Helvetica chimica acta》1995,78(5):1079-1082
Irradiation (λ > 390 nm) of 2H-1-benzothiopyran-2-one ( 1 ) in the solid state affords selectively 6aα,6bα,12bα,12cα -tetrahydrocyclobuta[1,2-c:4,3-c′]bis[1]benzothiopyran -6,7-dione ( 2 ), the head-to-head (HH) cis-cisoid-cis-dimer, while irradiation of 1 in the solid state using shorter wavelengths (λ > 340 nm) affords a mixture of all four cis-fused tricyclic dimers 2 – 5 . These results represent a novel wavelength effect in solid-state photochemistry. 相似文献