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121.
Benedikt J. L. Witzel Wilhelm Klein Jasmin V. Dums Marina Boyko Thomas F. Fssler 《Angewandte Chemie (International ed. in English)》2019,58(37):12908-12913
Endohedral clusters count as molecular models for intermetallic compounds—a class of compounds in which bonding principles are scarcely understood. Herein we report soluble cluster anions with the highest charges on a single cluster to date. The clusters reflect the close analogy between intermetalloid clusters and corresponding coordination polyhedra in intermetallic compounds. We now establish Raman spectroscopy as a reliable probe to assign for the first time the presence of discrete, endohedrally filled clusters in intermetallic phases. The ternary precursor alloys with nominal compositions “K5Co1.2Ge9” and “K4Ru3Sn7” exhibit characteristic bonding modes originating from metal atoms in the center of polyhedral clusters, thus revealing that filled clusters are present in these alloys. We report also on the structural characterization of [Co@Ge9]5? ( 1a ) and [Ru@Sn9]6? ( 2a ) obtained from solutions of the respective alloys. 相似文献
122.
Jasmin Dülfer Hao Yan Maxim N. Brodmerkel Robert Creutznacher Alvaro Mallagaray Thomas Peters Carl Caleman Erik G. Marklund Charlotte Uetrecht 《Molecules (Basel, Switzerland)》2021,26(8)
Noroviruses are the major cause of viral gastroenteritis and re-emerge worldwide every year, with GII.4 currently being the most frequent human genotype. The norovirus capsid protein VP1 is essential for host immune response. The P domain mediates cell attachment via histo blood-group antigens (HBGAs) in a strain-dependent manner but how these glycan-interactions actually relate to cell entry remains unclear. Here, hydrogen/deuterium exchange mass spectrometry (HDX-MS) is used to investigate glycan-induced protein dynamics in P dimers of different strains, which exhibit high structural similarity but different prevalence in humans. While the almost identical strains GII.4 Saga and GII.4 MI001 share glycan-induced dynamics, the dynamics differ in the emerging GII.17 Kawasaki 308 and rare GII.10 Vietnam 026 strain. The structural aspects of glycan binding to fully deamidated GII.4 P dimers have been investigated before. However, considering the high specificity and half-life of N373D under physiological conditions, large fractions of partially deamidated virions with potentially altered dynamics in their P domains are likely to occur. Therefore, we also examined glycan binding to partially deamidated GII.4 Saga and GII.4 MI001 P dimers. Such mixed species exhibit increased exposure to solvent in the P dimer upon glycan binding as opposed to pure wildtype. Furthermore, deamidated P dimers display increased flexibility and a monomeric subpopulation. Our results indicate that glycan binding induces strain-dependent structural dynamics, which are further altered by N373 deamidation, and hence hint at a complex role of deamidation in modulating glycan-mediated cell attachment in GII.4 strains. 相似文献
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124.
Jona Merx Kas J. Houthuijs Dr. Hidde Elferink Eva Witlox Dr. Jasmin Mecinović Prof. Jos Oomens Dr. Jonathan Martens Dr. Thomas J. Boltje Prof. Floris P. J. T. Rutjes 《Chemistry (Weinheim an der Bergstrasse, Germany)》2022,28(9):e202104078
N-Acyliminium ions are highly reactive intermediates that are important for creating CC-bonds adjacent to nitrogen atoms. Here we report the characterization of cyclic N-acyliminium ions in the gas phase, generated by collision induced dissociation tandem mass spectrometry followed by infrared ion spectroscopy using the FELIX infrared free electron laser. Comparison of DFT calculated spectra with the experimentally observed IR spectra provided valuable insights in the conformations of the N-acyliminium ions. 相似文献
125.
Christopher Reinknecht Anthony Riga Jasmin Rivera David A. Snyder 《Molecules (Basel, Switzerland)》2021,26(5)
Proteins are molecular machines requiring flexibility to function. Crystallographic B-factors and Molecular Dynamics (MD) simulations both provide insights into protein flexibility on an atomic scale. Nuclear Magnetic Resonance (NMR) lacks a universally accepted analog of the B-factor. However, a lack of convergence in atomic coordinates in an NMR-based structure calculation also suggests atomic mobility. This paper describes a pattern in the coordinate uncertainties of backbone heavy atoms in NMR-derived structural “ensembles” first noted in the development of FindCore2 (previously called Expanded FindCore: DA Snyder, J Grullon, YJ Huang, R Tejero, GT Montelione, Proteins: Structure, Function, and Bioinformatics 82 (S2), 219–230) and demonstrates that this pattern exists in coordinate variances across MD trajectories but not in crystallographic B-factors. This either suggests that MD trajectories and NMR “ensembles” capture motional behavior of peptide bond units not captured by B-factors or indicates a deficiency common to force fields used in both NMR and MD calculations. 相似文献
126.
Berry pomace, rich in polyphenols, especially anthocyanins, accumulates during the production of red juices. Pomace from chokeberry (Aronia melanocarpa Michx.), bilberry (Vaccinium myrtillus L.), and elderberry (Sambucus nigra L.) represent good sources of coloring foodstuffs. Pomace powders (PP) were prepared by milling the seedless fractions of the three dried berry pomaces (50 °C, 8 h). Techno-functional properties of the powders such as particle size distribution, bulk density, sedimentation velocity, and swelling capacity were determined to evaluate the powders for possible food applications. Total anthocyanin content was quantified by UHPLC-DAD before and during a storage experiment to monitor the degradation of anthocyanins in the PP and in a yogurt model application. The high content of phenolic compounds and the still intact cell structure ensured high stability of anthocyanins over 28 days of storage. In the model application, color saturation was stable over the whole storage time of 14 days. Regarding the techno-functional properties, only a few differences between the three PP were observed. The particle size of elderberry PP was larger, resulting in lowest bulk density (0.45 g/mL), high cold-water solubility (16.42%), and a swelling capacity of 10.16 mL/g dw. Sedimentation velocity of the three PP was fast (0.02 mL/min) due to cluster formation of the particles caused by electrostatic and hydrophobic properties. Compared to other high-intensity coloring foodstuffs, the use of PP, showing acceptable color stability with potential health-promoting effects, represents a wide applicability in different food applications and especially in products with a longer shelf-life. 相似文献
127.
Jasmin Shah M. Rasul Jan Sultan Shah S. Niaz Ali Shah 《Journal of Analytical Chemistry》2014,69(7):638-645
A simple, precise and sensitive spectrofluorimetric method was developed for the determination of cephradine in pharmaceutical formulations. The method is based on reaction of cephradine with ethyl acetoacetate (EAA) in the presence of formaldehyde in acidic media. The fluorescence intensity of the resultant fluorescent derivative was measured at 443 nm after excitation at 350 nm. The effects of various experimental parameters on the formation of the fluorescent product were studied and optimized. A linear relationship between concentration of cephradine and fluorescence intensity was found over the range of 0.1–5.0 μg/mL. The limit of detection and quantification were calculated an found 1.09 × 10?2 ± 3.64 × 10?3 μg/mL and 3.64 × 10?2 ± 3.64 × 10?3 μg/mL, respectively and with relative standard deviation (RSD) 4.14%. Accuracy of the method was checked by standard addition method and applied to four different commercial formulations. The percentage recovery was found in the range of 97.03 to 103.80% for Velora suspension, 98.16 to 102.90% for velocef injection, 99.00 to 108.10% for Velora capsule and 99.06 to 104.90% for Cefradin capsule. The good percentage recoveries from all samples indicated that there were no interferences from the common excipients of formulations. The proposed method was successfully applied to the analysis of commercial suspension, capsule and injections. The result obtained by the proposed method was statistically validated with reference HPLC method. No significant difference in the results of the two methods was found regarding accuracy and precision using Student’s t-test and the variance ratio F-test. 相似文献
128.
129.
Muhammad Naeem Khan Jasmin Shah Muhammad Rasul Jan Sang Hak Lee 《Journal of fluorescence》2013,23(1):161-169
A simple, sensitive, and accurate spectrofluorimetric method was developed for the determination of citalopram in bulk and pharmaceutical preparations. The method is based on the enhancement of the weak fluorescence signal (FL) of the Tb (III)-citalopram system in the presence of silver nanoparticles. Fluorescence intensities were measured at 555 nm after excitation at 281 nm. Prepared silver nanoparticles (AgNPs) were characterized by UV-Visible spectra and transmission electron microscopy (TEM). Various factors affecting the formation of citalopram-Tb (III)-AgNPs complexes were studied and optimized. The fluorescence intensity versus concentration plot was linear over the range 0.02–14 μg?mL?1, with an excellent correlation coefficient of 0.9978. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 7.15?×?10?6?μg?mL?1 and 2.38?×?10?5?μg?mL?1 respectively. The proposed method was found to have good reproducibility with a relative standard deviation of 3.66 % (n?=?6). The interference effects of common excipients found in pharmaceutical preparations were studied. The developed method was validated statistically by performing recoveries studies and successfully applied for the assay of citalopram in bulk powder and pharmaceutical preparations. Percent recoveries were found to range from 98.98 % to 100.97 % for bulk powder and from 96.57 % to 101.77 % for pharmaceutical preparations. 相似文献
130.
A quick and highly efficient microwave-assisted preparation of imidazopyridines and –quinolines is described, starting from the corresponding ketones and amines. The method requires no solvent and uses activated MnO2 as an oxidant. A mechanism for the cyclization is proposed and discussed. 相似文献