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1.
Dr. Miguel Cortijo Dr. Ángela Valentín-Pérez Dr. Andrei Rogalev Dr. Fabrice Wilhelm Dr. Philippe Sainctavit Dr. Patrick Rosa Dr. Elizabeth A. Hillard 《Chemistry (Weinheim an der Bergstrasse, Germany)》2020,26(59):13363-13366
An original method for determining the handedness of individual non-centrosymmetric crystals in a mixture using a tightly-focused, circularly polarized X-ray beam is presented. The X-ray natural circular dichroism (XNCD) spectra recorded at the metal K-edge on selected crystals of [Δ-M(en)3](NO3)2 and [Λ-M(en)3](NO3)2 (M=CoII, NiII) show extrema at the metal pre-edge (7712 eV for Co, 8335 eV for Ni). A mapping of a collection of some 220 crystals was performed at the respective energies by using left and right circular polarizations. The difference in absorption for the two polarizations, being either negative or positive, directly yielded the handedness of the crystal volume probed by the beam. By using this technique, it was found that the addition of l -ascorbic acid during the synthesis of [Co(en)3](NO3)2 resulted in an enantiomeric enrichment of the Λ-isomer of 67±13 %, whereas the Ni analogue was similarly, but conversely, enriched in the Δ-isomer (65±22 %). 相似文献
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Gatto Claudia C. Chagas Marcio A. S. Lima Iariane J. Mello Andrade Francyelli Silva Hugo D. Abrantes Gabrielly R. Lacerda Elisângela P. S. 《Transition Metal Chemistry》2019,44(4):329-340
Transition Metal Chemistry - The present study reports the synthesis and crystal structures of Cu(II) complexes with pyridoxal S-allyldithiocarbazate (H2L1) and pyridoxal thiosemicarbazones... 相似文献
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Influence of the Solvent on the “Casting” Methodology for MWCNT‐Modified Glassy Carbon and Platinum Electrodes 下载免费PDF全文
Ana Carolina Ângelo Dorim Herbert Aleixo Edilton de Souza Barcellos Leonardo Luiz Okumura 《Electroanalysis》2015,27(11):2663-2669
The choice of electrode material and surface preparation method are usually dictated by the suitability of the electrode to observe an electrochemical parameter, such as heterogeneous electron transfer rate, surface coverage, or redox potential. Thus, the glassy carbon (GC) and platinum (Pt) electrodes were modified with multiwalled carbon nanotubes (MWCNT) by direct “casting” modification using nine different aliquots of solvents. After drying at room temperature, the modified electrode showed distinct redox peaks corresponding to ferrocyanide oxidation/reduction. Using chemometrics, the cyclic voltammograms with higher current intensity were obtained for those in which ethanol, water and acetone as dispersing agents were used for GCE and dimethylformamide, water and acetone for Pt electrode modification. 相似文献
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Prof. Javier Ruiz Lucía García Dr. Marilín Vivanco Ángela Berros Dr. Juan Francisco Van der Maelen 《Angewandte Chemie (International ed. in English)》2015,54(14):4212-4216
By means of a combined experimental and theoretical approach, the electronic features and chemical behavior of metalla‐N‐heterocyclic carbenes (MNHCs, N‐heterocyclic carbenes containing a metal atom within the heterocyclic skeleton) have been established and compared with those of classical NHCs. MNHCs are strongly basic (proton affinity and pKa values around 290 kcal mol?1 and 36, respectively) with a narrow singlet–triplet gap (around 23 kcal mol?1). MNHCs can be generated from the corresponding metalla‐imidazolium salts and trapped by addition of transition‐metal complexes affording the corresponding heterodimetallic dicarbene derivatives, which can serve as carbene transfer agents. 相似文献
5.
Pedro Rocha ngela Vilas‐Boas Natacha Fontes Dulce Geraldo Ftima Bento 《Electroanalysis》2020,32(1):159-165
The electrochemical oxidation processes that occur during a voltammetric assay in wine samples lead to the formation of species that obstructs the surface and reduce their active area. This effect is critical for screen printed carbon electrodes (SPCE) and leads to abnormal low values of the total polyphenols content of wines, ca. 72 % lower than those obtained with glassy carbon electrodes. This effect was examined using 10 red and Port wine samples. Mechanical polishing and electrochemical‐based treatments for the removal of this fouling layer were tested. The best results were obtained by electrochemical activation in at a constant potential of 1.2 V during 100 s Na2CO3 saturated solution, and by polishing. The success of some of these treatments brings an added value to SPCE, as it opens the possibility of their reuse in the wine analysis. This outcome is particularly relevant for quality control where a huge number of analysis is performed and the reduction of cost may dictates the choice of the analytical method. 相似文献
6.
Rapid and sensitive ultra‐high‐pressure liquid chromatography method for quantification of antichagasic benznidazole in plasma: application in a preclinical pharmacokinetic study 下载免费PDF全文
Marcelo Gomes Davanço Michel Leandro de Campos Rosângela Gonçalves Peccinini 《Biomedical chromatography : BMC》2015,29(7):1008-1015
Benznidazole (BNZ) and nifurtimox are the only drugs available for treating Chagas disease. In this work, we validated a bioanalytical method for the quantification of BNZ in plasma aimed at improving sensitivity and time of analysis compared with the assays already published. Furthermore, we demonstrated the application of the method in a preclinical pharmacokinetic study after administration of a single oral dose of BNZ in Wistar rats. A Waters® Acquity UHPLC system equipped with a UV–vis detector was employed. The method was established using an Acquity® UHPLC HSS SB C18 protected by an Acquity® UHPLC HSS SB C18 VanGuard guard column and detection at 324 nm. The mobile phase consisted of ultrapure water–acetonitrile (65:35), and elution was isocratic. The mobile phase flow rate was 0.55 mL/min, the volume of injection was 1 μL, and the run time was just 2 min. The samples were kept at 25°C until injection and the column at 45°C for the chromatographic separation. The sample preparation was performed by a rapid protein precipitation with acetonitrile. The linear concentration range was 0.15–20 µg/mL. The pharmacokinetic parameters of BNZ in rats were determined and the method was considered sensitive, fast and suitable for application in pharmacokinetic studies. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
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Dr. Steffen Bähring Dr. Luis Martín‐Gomis Gunnar Olsen Prof. Dr. Kent A. Nielsen Dr. Dong Sub Kim Dr. Troels Duedal Prof. Dr. Ángela Sastre‐Santos Prof. Dr. Jan O. Jeppesen Prof. Dr. Jonathan L. Sessler 《Chemistry (Weinheim an der Bergstrasse, Germany)》2016,22(6):1958-1967
Supramolecular polymers are a class of macromolecules stabilized by weak non‐covalent interactions. These self‐assembled aggregates typically undergo stimuli‐induced reversible assembly and disassembly. They thus hold great promise as so‐called functional materials. In this work, we present the design, synthesis, and responsive behavior of a short supramolecular oligomeric system based on two hetero‐complementary subunits. These “monomers” consist of a tetrathiafulvalene‐functionalized calix[4]pyrrole (TTF‐C[4]P) and a glycol diester‐linked bis‐2,5,7‐trinitrodicyanomethylenefluorene‐4‐carboxylate (TNDCF), respectively. We show that when mixed in organic solvents, such as CHCl3, CH2ClCH2Cl, and methylcyclohexane, supramolecular aggregation takes place to produce short oligomers stabilized by hydrogen bonding and donor–acceptor charge‐transfer (CT) interactions. The self‐associated materials were characterized by 1H NMR and UV/Vis/NIR absorption spectroscopy, as well as by concentration‐ and temperature‐dependent absorption spectroscopy and dynamic light scattering (DLS) analyses of both the monomeric and oligomerized species. The self‐associated system produced from TTF‐C[4]P and TNDCF exhibits a concentration‐dependent aggregation behavior typical of supramolecular polymers. Further support for the proposed self‐assembly came from theoretical calculations. The fluorescence emitting properties of TNDCF are quenched under conditions that promote the formation of supramolecular aggregates containing TTF‐C[4]P and TNDCF. This quenching effect has been utilized as a probe for the detection of substrates in the form of anions (i.e., chloride) and nitroaromatic explosives (i.e., 1,3,5‐trinitrobenzene). Specifically, the addition of these substrates to mixtures of TTF‐C[4]P and TNDCF produced a fluorescence “turn‐on” response. 相似文献
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The lipase catalyzed resolution of trans-3,4-tetrahydrofuran and pyrrolidine bromohydrins by acylation or hydrolysis of their acylated derivatives has been studied. For both heterocycles, the best enantioselectivity was obtained using Candida antarctica lipase B as the catalyst in the hydrolytic processes. The enantiomerically pure bromohydrins are useful intermediates for the preparation of 3,4-fuctionalized cis-heterocycles. 相似文献
10.
Ângelo M.L. Denadai André M. de Oliveira Izabela M.P. Daniel Luan A. Carneiro Kherolayne C. Ribeiro Heloísa de O. Beraldo 《Supramolecular chemistry》2013,25(3):204-212
Chlorhexidine is a widely used, di-cationic, broad-spectrum antimicrobial agent and losartan is a well-known, anionic-specific antagonist of AT1 renin–angiotensin receptor that acts as an anti-hypertensive agent. The combination of these molecules gives a chlorhexidine di-losartanate (ClxLos2) hydrophobic ion pair that spontaneously aggregates into nanoparticles (NPs). This work investigated the formation of ClxLos2 NPs using the analysis of the solid state by fourier transform infrared spectroscopy, thermogravimetric analysis, differential scanning calorimetry and scanning electron microscopy and in aqueous environment by calorimetric, zeta potential and dynamic light scattering titrations. Furthermore, to demonstrate the potential antimicrobial activity of ClxLos2, in vitro antibacterial tests were conducted against Staphylococcus aureus (ATCC 27664), Streptococcus viridans (ATCC 11563) and Enterococcus faecalis (ATCC 14508). Based on these studies, it is proposed that ClxLos2 could be used for controlled drug release based on ionic dissociation during dilution, thereby avoiding the use of any solid matrix. 相似文献