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21.
Edison SE Lin LA Gamble BM Wong J Zhang K 《Rapid communications in mass spectrometry : RCM》2011,25(1):127-139
A rapid screening method for pesticides has been developed to promote more efficient processing of produce entering the United States. Foam swabs were used to recover a multiclass mixture of 132 pesticides from the surfaces of grapes, apples, and oranges. The swabs were analyzed using direct analysis in real time (DART) ionization coupled with a high‐resolution Exactive Orbitrap? mass spectrometer. By using a DART helium temperature gradient from 100–350°C over 3 min, a minimal separation of analytes based on volatility differences was achieved. This, combined with the Exactive's mass resolution of 100 000, allowed the chromatographic step, along with the typical compositing and extraction steps associated with gas chromatography/mass spectrometry (GC/MS) or liquid chromatography/mass spectrometry (LC/MS) approaches, to be eliminated. Detection of 86% of the analytes present was consistently achieved at levels of 2 ng/g (per each apple or orange) and 10 ng/g (per grape). A resolution study was conducted with four pairs of isobaric compounds analyzed at a mass resolution of 100 000. Baseline separation was achieved with analyte ions differing in mass by 25 ppm and analyte ions with a mass difference of 10 ppm were partially resolved. In addition, field samples that had undergone traditional sample preparation using QuEChERS (quick, easy, cheap, rugged, and safe) were analyzed using both LC/MS and DART‐MS and the results from the two techniques were found to be comparable in terms of identification of the pesticides present. The use of swabs greatly increased sample throughput by reducing sample preparation and analysis time. Published in 2010 by John Wiley & Sons, Ltd. 相似文献
22.
Dolashka P Moshtanska V Dolashki A Velkova L Rao GS Angelova M Betzel C Voelter W Atanasov B 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2011,83(1):67-73
The native form of Cu/Zn-superoxide dismutase, isolated from fungal strain Humicola lutea 103 is a homodimer that coordinates one Cu(2+) and one Zn(2+) per monomer. Cu(2+) and Zn(2+) ions play crucial roles in enzyme activity and structural stability, respectively. It was established that HLSOD shows high pH and temperature stability. Thermostability of the glycosylated enzyme Cu/Zn-SOD, isolated from fungal strain H. lutea 103, was determined by CD spectroscopy. Determination of reversibility toward thermal denaturation for HLSOD allowed several thermodynamic parameters to be calculated. In this communication we report the conditions under which reversible denaturation of HLSOD exists. The narrow range over which the system is reversible has been determined using the strongest test of two important thermodynamic independent variables (T and pH). Combining both these variables, the "phase diagram" was determined, as a result of which the real thermodynamic parameters (ΔC(p), ΔH(exp)°, and ΔG(exp)°) was established. Because very narrow pH-interval of transitions we assume they are as result of overlapping of two simple transitions. It was found that ΔH(o) is independent from pH with a value of 1.3 kcal/mol and 2.8 kcal/mol for the first and the second transition, respectively. ΔG(o) was pH-dependent in all studied pH-interval. This means that the transitions are entropically driven, these. Based on this, these processes can be described as hydrophobic rearrangement of the quaternary structure. It was also found that glycosylation does not influence the stability of the enzyme because the carbohydrate chain is exposed on the surface of the molecule. 相似文献
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24.
Polina Angelova Kalina Kostova Karsten Hinrichs Dimiter Tsankov 《Central European Journal of Chemistry》2005,3(4):658-667
New 4-substituted benzyl esters of 16-mercaptohexadecanoic acid were prepared by developing a practicable synthetic procedure
and using readily available staring materials. The compounds synthesized have been characterized by NMR, MS, IR spectra and
elemental analysis. The mercapto derivatives are precursors for the formation of self-assembled monolayers on metal substrates.
Dedicated to Professor Dr. Manfred Hesse on the occasion of his 70
th
birthday 相似文献
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In this paper, we consider large‐scale nonsymmetric differential matrix Riccati equations with low‐rank right‐hand sides. These matrix equations appear in many applications such as control theory, transport theory, applied probability, and others. We show how to apply Krylov‐type methods such as the extended block Arnoldi algorithm to get low‐rank approximate solutions. The initial problem is projected onto small subspaces to get low dimensional nonsymmetric differential equations that are solved using the exponential approximation or via other integration schemes such as backward differentiation formula (BDF) or Rosenbrock method. We also show how these techniques can be easily used to solve some problems from the well‐known transport equation. Some numerical examples are given to illustrate the application of the proposed methods to large‐scale problems. 相似文献
28.
Yan-Cen Liu Dr. Shu Peng Lora Angelova Prof. Dr. Werner M. Nau Dr. Andreas Hennig 《ChemistryOpen》2019,8(11):1350-1354
The combination of the macrocyclic hosts p-sulfonatocalix[4]arene and cucurbit[7]uril with the fluorescent dyes lucigenin and berberine affords two label-free enzyme assays for the detection of kinase and phosphatase activity by fluorescence monitoring. In contrast to established assays, no substrate labeling is required. Since phosphorylation is one of the most important regulatory mechanisms in biological signal transduction, the assays should be useful for identification of inhibitors and activators in high-throughput screening (HTS) format for drug discovery. 相似文献
29.
O. Angelova J. Macicek N. G. Vassilev S. Momchilova J. Petrova 《Journal of chemical crystallography》1992,22(3):253-258
The crystal structures of threo(RR,SS) diethyl ester of 2-hydroxy-1,2-diphenylethylphosphonic acid (1) and of (±)diethyl ester of (1-hydroxycyclopentyl)(2-methylphenyl)methylphosphonic acid (2) have been solved by X-ray methods. They are built up in a similar way to centrosymmetric dimers of hydrogen-bonded molecules. The orientation of the substituents around the central C-C bond in both molecules fulfills the requirement for the least spatial hindrance. The observed shift of the
oh stretching frequencies from 3312(1), 3346 (2) cm–1 in solid to 3408(1), 3450(2), in diluted (10–3
M) tetrachloromethane solution, indicates the formation of intramolecular hydrogen-bonded species. 相似文献
30.
García Martínez A de la Moya Cerero S Teso Vilar E García Fraile A Lora Maroto B Díaz Morillo C 《The Journal of organic chemistry》2008,73(17):6607-6614
The study of the stereochemical outcome of the solvolysis of oxaspirocyclopropanated 1-norbornyl triflates is highly interesting since these reactions do not lead to the usual retention or fragmentation products but only synthetically interesting rearranged products are enantiospecifically formed. There is no correlation between the experimental solvolysis rates (ln k) and the B3LYP/6-31G(d)-computed ionization energies (Delta E) of the corresponding bridgehead hydrocarbons in gas phase. However, this work demonstrates the existence of a fair linear correlation between the experimental reaction rates and the PCM//B3LYP/6-31G(d)-computed free ionization energies in solution (Delta G). This theoretically relevant result reveals that the reason for the lack of linearity in gas phase is not the rearrangement of the intermediate carbocations but unspecific solvent effects on the solvolysis rates, accounted for by the PCM model. 相似文献