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71.
Evgenyi V. Gryshkun Natalia V. Andrushko Oleg I. Kolodiazhnyi 《Phosphorus, sulfur, and silicon and the related elements》2013,188(6):1027-1046
Racemic chlorophosphines react stereoselectively with chiral l-phenylethylamines or amino acid esters to give diastereomerically enriched aminophosphines 3, which were isolated as diastereomerically pure crystalline borane complexes. Oxidation, thionation, the reaction with methyl iodide provide optically active derivatives of aminophosphines. (R,S)- and (S,S)-stereomers of phosphinic acid amides were separated by crystallization and a flash-chromatography. The stereochemical properties of phosphorus acid amides were investigated. The mechanism of asymmetric induction at the trivalent phosphorus atom was rationalized. 相似文献
72.
Anatoli Tchigvintsev Dmitri Tchigvintsev Robert Flick Ana Popovic Aiping Dong Xiaohui Xu Greg Brown Wenyun Lu Hong Wu Hong Cui Ludmila Dombrowski Jeong Chan Joo Natalia Beloglazova Jinrong Min Alexei Savchenko Amy A. Caudy Joshua D. Rabinowitz Alexey G. Murzin Alexander F. Yakunin 《Chemistry & biology》2013,20(11):1386-1398
73.
Alexander Boichenko Natalia Govorukhina Ate G. J. van der Zee Rainer Bischoff 《Analytical and bioanalytical chemistry》2013,405(10):3195-3203
Macroporous reversed-phase (mRP) chromatography was successfully used to develop an accurate and precise method for total protein in serum. The limits of detection (0.83 μg, LOD) and quantification (2.51 μg, LOQ) for the mRP method are comparable with those of the widely used micro BCA protein assay. The mRP method can be used to determine the total protein concentration across a wide dynamic range by detecting chromatographic peaks at 215 nm and 280 nm. The method has the added advantage of desalting and denaturing proteins, leading to more complete digestion by trypsin and to better LC–MS–MS identification in shotgun proteomics experiments. Figure
Simultaneous Serum Desalting and Total Protein Determination with Macroporous Reversed-Phase Chromatography: calibration plots 相似文献
74.
Natalia P. Ivleva Susanne Huckele Bernadett Weinzierl Reinhard Niessner Christoph Haisch Thomas Baumann 《Analytical and bioanalytical chemistry》2013,405(28):9071-9084
We present for the first time the Raman microspectroscopic identification and characterization of individual airborne volcanic ash (VA) particles. The particles were collected in April/May 2010 during research aircraft flights, which were performed by Deutsches Zentrum für Luft- und Raumfahrt in the airspace near the Eyjafjallajökull volcano eruption and over Europe (between Iceland and Southern Germany). In addition, aerosol particles were sampled by an Electrical Low Pressure Impactor in Munich, Germany. As references for the Raman analysis, we used the spectra of VA collected at the ground near the place of eruption, of mineral basaltic rock, and of different minerals from a database. We found significant differences in the spectra of VA and other aerosol particles (e.g., soot, nitrates, sulfates, and clay minerals), which allowed us to identify VA among other atmospheric particulate matter. Furthermore, while the airborne VA shows a characteristic Raman pattern (with broad band from ca. 200 to ca. 700 cm?1 typical for SiO2 glasses and additional bands of ferric minerals), the differences between the spectra of aged and fresh particles were observed, suggesting differences in their chemical composition and/or structure. We also analyzed similarities between Eyjafjallajökull VA particles collected at different sampling sites and compared the particles with a large variety of glassy and crystalline minerals. This was done by applying cluster analysis, in order to get information on the composition and structure of volcanic ash. Figure
Images and Raman spectra of airborne volcanic ash 相似文献
75.
Manuel Sergi Natalia Battista Camilla Montesano Roberta Curini Mauro Maccarrone Dario Compagnone 《Analytical and bioanalytical chemistry》2013,405(2-3):785-793
Endocannabinoids (ECs) are endogenous compounds that interact with type-1 and type-2 cannabinoid receptors (CB1 and CB2), as well as non-cannabinoid receptors. The multitude of roles attributed to ECs makes them an emerging target of pharmacotherapy for a number of disparate diseases. Here a high-throughput bioanalytical method based on micro SPE (μ-SPE) followed by LC-MS/MS analysis for the simultaneous determination of the two major endocannabinoids 2-arachidonoylglycerol (2-AG) and N-arachidonoylethanolamine (anandamide, AEA) in human plasma is presented. The chromatographic conditions obtained with the fused-core column allowed a good separation in 10 min also of the AG isomers. A very simple and reliable extraction has been optimised by means of C18-modified tips: it requires only 100 μL of plasma and allows the use of minimal volumes of organic solvent. The present method allows a rapid and effective clean-up, which also minimises the isomerisation of 2-AG. The whole procedure has been validated following the FDA guidelines for bioanalytical methods validation: the satisfactory recovery values, the negligible matrix effect and the good values of accuracy and reproducibility make it a simple and high-throughput analytical tool for clinical and biochemical studies on endocannabinoid signaling in humans. Figure
Determination of the two major endocannabinoids in human plasma by μ-SPE followed by HPLC-MS/MS 相似文献
76.
Hyeran Lee Mikhail Y. Berezin Rui Tang Natalia Zhegalova Samuel Achilefu 《Photochemistry and photobiology》2013,89(2):326-331
Near‐infrared heptamethine cyanine dye is functionalized with pyrazole derivatives at the meso‐position to induce pH‐dependent photophysical properties. The presence of pyrazole unsubstituted at 1N‐position is essential to induce pH‐dependent fluorescence intensity and lifetime changes in these dyes. Replacement of meso‐chloro group of cyanine dye IR820 with 1N‐unsubstituted pyrazole resulted in the pH‐dependent fluorescence lifetime changes from 0.93 ns in neutral media to 1.27 ns in acidic media in DMSO. Time‐resolved emission spectra (TRES) revealed that at lower pH, the pyrazole consists of fluorophores with two distinct lifetimes, which cor‐responds to pH‐sensitive and non‐pH‐sensitive species. In contrast, 1N‐substituted pyrazoles do not exhibit pH response, suggesting excited state electron transfer as the mechanism of pH‐dependent fluorescence lifetime sensitivity for this class of compounds. 相似文献
77.
Natalia Ríos Cecilia Chavarría Carmen Gil Williams Porcal 《Journal of heterocyclic chemistry》2013,50(3):720-726
An efficient and rapid microwave‐assisted solid‐phase method for the synthesis of 5‐methyl‐1,2‐disubstituted benzimidazoles derivatives has been developed. The phosphonium linker, obtained by reaction between polymer‐supported triphenylphosphine and 4‐fluoro‐3‐nitrobenzyl iodide, underwent aromatic substitution with primary amines, followed by one‐pot reaction with aldehydes in the presence of SnCl2·2H2O, yielded the benzimidazole system under microwave irradiation. The final products were released from the resin with NaOH under microwave irradiation and were obtained in high purity and good overall yield. 相似文献
78.
Ricardo C. Pasquali Natalia Sacco Carlos Bregni 《Journal of Dispersion Science and Technology》2013,34(4):479-481
In this article, we obtained equations that permit us to calculate the hydrophilic-lipophilic balance (HLB) value of polyoxyethylene esters from quality control data of the raw materials (fatty acids and polyethylene glycol) and the finished product (surfactant). These data include the acid value of the fatty acid, the hydroxyl value of the polyethylene glycol, and the hydroxyl value of the surfactant. These calculations permit us, moreover, to know the mean molecular masses of fatty acids, of polyethylene glycol, of monoester and diester, and the proportion of polyoxyethylene monoester and polyoxyethylene diester. 相似文献
79.
Niko Kivel Natalia Shcherbina Ines Günther-Leopold 《Journal of Radioanalytical and Nuclear Chemistry》2013,296(1):557-561
Novel reprocessing schemes and techniques are the focus of the Euratom FP7 project “Actinide Recycling for Separation and Transmutation” (ACSEPT), where the Paul Scherrer Institute (PSI) is represented in the pyrochemical domain. The subject of investigation is the selective separation of fission products (FPs) from spent nuclear fuel as a head-end step to either classical hydro based or pyro processes which are not yet applied on a large scale. The selective removal of FPs that are major contributors to the overall radiation dose or bear great potentials in terms of radiotoxicity (i.e. cesium or iodine), is advantageous for further processes. At PSI a device was developed to release volatile FPs by means of inductive heating. The heating up to 2,300 °C promotes the release of material that is further transported by a carrier gas stream into an inductively coupled plasma mass spectrometer for online detection. The carrier gas can be either inert (Ar) or can contain reducing or oxidizing components like hydrogen or oxygen, respectively. The development of the device by computer aided engineering approaches, the commissioning and evaluation of the device and data from first release experiments on a simulated fuel matrix are discussed. 相似文献
80.
Tyler T. Clikeman Dr. Igor V. Kuvychko Dr. Natalia B. Shustova Dr. Yu‐Sheng Chen Dr. Alexey A. Popov Dr. Olga V. Boltalina Prof. Steven H. Strauss 《Chemistry (Weinheim an der Bergstrasse, Germany)》2013,19(16):5070-5080
The sequential addition of CN? or CH3? and electrophiles to three perfluoroalkylfullerenes (PFAFs), Cs‐C70(CF3)8, C1‐C70(CF3)10, and Cs‐p‐C60(CF3)2, was carried out to determine the most reactive individual fullerene C atoms (as opposed to the most reactive C?C bonds, which has previously been studied). Each PFAF reacted with CH3? or CN? to generate metastable PFAF(CN)? or PFAF(CH3)22? species with high regioselectivity (i.e., one or two predominant isomers). They were treated with electrophiles E+ to generate PFAF(CN)(E) or PFAF(CH3)2(E)2 derivatives, also with high regioselectivity (E+=CN+, CH3+, or H+). All of the predominant products, characterized by mass spectrometry and 19F NMR spectroscopy, are new compounds. Some could be purified by HPLC to give single isomers. Two of them, C70(CF3)8(CN)2 and C70(CF3)10(CH3)2(CN)2, were characterized by single‐crystal X‐ray diffraction. DFT calculations were used to propose whether a particular reaction is under kinetic or thermodynamic control. 相似文献