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141.
A number of 4,5‐dichloro‐ and 4,5‐dibromopyridazin‐3‐ones and ‐3,6‐diones with polyfluoro substituents at position 2 were obtained in good yields by microwave‐assisted method. The oxopyridazines as well as their respective 5‐dimethylaminoethylamino derivatives were tested for antibacterial, antiviral, and antiprotozoal activity. 相似文献
142.
J. Morais M. A. Pérez‐de la Rosa 《Mathematical Methods in the Applied Sciences》2015,38(17):4365-4387
Over the past few years, considerable attention has been given to the role played by the Lamé's Wave Functions (LWFs) in various problems of mathematical physics and mechanics. The LWFs arise via the method of separation of variables for the wave equation in ellipsoidal coordinates. The present paper introduces the Lamé's Quaternionic Wave Functions (LQWFs), which extend the LWFs to a non‐commutative framework. We show that the theory of the LQWFs is determined by the Moisil‐Theodorescu type operator with quaternionic variable coefficients. As a result, we explain the connections between the solutions of the Lamé's wave equation, on one hand, and the quaternionic hyperholomorphic and anti‐hyperholomorphic functions on the other. We establish analogues of the basic integral formulas of complex analysis such as Borel‐Pompeiu's, Cauchy's, and so on, for this version of quaternionic function theory. We further obtain analogues of the boundary value properties of the LQWFs such as Sokhotski‐Plemelj formulae, the ‐hyperholomorphic extension of a given Hölder function and on the square of the singular integral operator. We address all the text mentioned earlier and explore some basic facts of the arising quaternionic function theory. We conclude the paper showing that the spherical, prolate, and oblate spheroidal quaternionic wave functions can be generated as particular cases of the LQWFs. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
143.
Belén Abarca Rafael Ballesteros Rosa Adam Rafael Ballesteros-Garrido Frédéric R. Leroux Françoise Colobert Ibon Alkorta José Elguero 《Tetrahedron》2014
A dynamic 1H NMR study, together with DFT calculations, of bis-([1,2,3]triazolo)[1,5-a:5′,1′-k][1,10]phenanthroline 2 has allowed to identify the ring and open forms of a new example of ring/chain tautomerism, as well as their interconversion barriers (ring/ring and ring/open). The barrier of the exchange process between the chain forms and the ring form was found higher than the ‘racemization’ process in the closed form, so the ring opening does not contribute to the ‘racemization’. The di-1,10-methyl and di-1,10-iodo derivatives have been prepared and their properties calculated. 相似文献
144.
Novel Fréchet–PAMAM hybrid dendrimers linked by triazole units as unimolecular micelles with a hydrophobic core surrounded by a hydrophilic shell were prepared. The dendritic cores with 3 and 6 alkyne terminal groups were synthesized from 1,3,5-tribromomethyl-benzene (tBrMeB), in one case by direct coupling with 17α-ethynylestradiol (EE); in the second one the tBrMeB was reacted with bis(hydroxymethyl) phenol followed by chlorination of the hydroxyl groups and subsequent coupling to EE. With this strategy, the core can be grown by further substitutions of bis(hydroxymethyl) phenol over the halogenated terminals as Fréchet dendrimer. The hydrophilic shells used were PAMAM type dendrons of 0.5 and 1.5 generations with azide as focal point and tert-butyl ester as end groups. The unimolecular micelles were obtained by cycloaddition between an azide in the selected dendron and the alkyne terminal in the hydrophobic core to obtain a 1,4-disubstituted 1,2,3-triazole. Once the coupling was achieved, the tert-butyl ester groups were hydrolyzed in trifluoroacetic acid and the corresponding dendrimers with carboxylic acid as end groups were completely soluble in phosphate buffer solutions of pH 7.0, 7.4, and 8.0. All hybrid dendrimers were characterized by High Resolution Mass Spectrometry, 1H and 13C NMR, and FTIR. 相似文献
145.
Ionic liquids as stationary phases in gas chromatography: Determination of chlorobenzenes in soils
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Rosa María González Paredes Carmelo García Pinto José Luis Pérez Pavón Bernardo Moreno Cordero 《Journal of separation science》2014,37(12):1448-1455
The present research focuses on the evaluation of different ionic liquid (IL) stationary phases in gas chromatography. The different IL columns were evaluated in terms of peak resolution (Rs) and peak symmetry for the separation of the chlorobenzenes. The determination of chlorobenzenes in soil samples by means of the optimal IL stationary phase (SLB‐IL82) is proposed as an application. Soil pretreatment was based on a simplified quick, easy, cheap, effective, rugged, and safe extraction procedure and a large injection volume via a programed temperature vaporizer working in solvent vent mode. The retention time of the chlorobenzenes increased as the polarity of the IL column decreased. SLB‐IL82 is the stationary phase that provides the best values as regards Rs and asymmetry factor. Soil sample blanks were spiked with the analytes before subjecting the sample to the extraction process. The existence of a matrix effect was checked and the analytical characteristics of the method were determined in a fortified garden soil sample. The method provided good linearity, good repeatability and reproducibility values, and the LODs were in the 0.1–4.7 μg/kg range. Two fortified soil samples were applied to validate the proposed methodology. 相似文献
146.
Study of the retention behavior of iodinated X‐ray contrast agents in hydrophilic interaction liquid chromatography,comparing bare silica and zwitterionic stationary phases
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Daniela Salas Francesc Borrull Rosa Maria Marcé Núria Fontanals 《Journal of separation science》2014,37(9-10):1111-1117
Iodinated X‐ray contrast media are the most widely used pharmaceuticals for intravascular administration in X‐ray diagnostic procedures. The increasing concern of the fate of these compounds into the environment has led to the development of analytical methods to determine them. However, these methods present problems due to the polar character of these analytes. In this paper, hydrophilic interaction LC is presented as an alternative technique. The retention of iodinated X‐ray contrast media was studied in two bare silica phases with different particle designs (i.e. porous and Fused Core?) and a zwitterionic sulfoalkylbetaine phase. The effect of the most important parameters of the mobile phase was studied for each stationary phase. It was observed that optimal mobile phase conditions included buffers with a high buffering capacity. Additionally, the retention mechanisms involved were studied in order to provide some insight into the possible occurring interactions. The contributions of partition and adsorption and the effect of the temperature on the retention of analytes were evaluated on all of the stationary phases. 相似文献
147.
A useful approach for the differentiation of wines according to geographical origin based on global volatile patterns
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In this study, the feasibility of solid‐phase extraction combined with gas chromatography and mass spectrometry in tandem with partial least squares discriminant analysis was evaluated as a useful strategy to differentiate wines according to geographical origin (Azores, Canary and Madeira Islands) and types (white, red and fortified wine) based on their global volatile patterns. For this purpose, 34 monovarietal wines from these three wine grape‐growing regions were investigated, combining the high throughput extraction efficiency of the solid‐phase extraction procedure with the separation and identification ability. The partial least squares discriminant analysis results suggested that Madeira wines could be clearly discriminated from Azores and Canary wines. Madeira wines are mainly characterized by 2‐ethylhexan‐1‐ol, 3,5,5‐trimethylhexan‐1‐ol, ethyl 2‐methylbutanoate, ethyl dl ‐2‐hydroxycaproate, decanoic acid, 3‐methylbutanoic acid, and (E)‐whiskey lactone, whereas 3‐ethoxypropan‐1‐ol, 1‐octen‐3‐ol, (Z)‐3‐hexenyl butanoate, 4‐(methylthio)‐1‐butanol, ethyl 3‐hydroxybutanoate, isoamyl lactate, 4‐methylphenol, γ‐octalactone and 4‐(methylthio)‐1‐butanol, are mainly associated with Azores and Canary wines. The data obtained in this study revealed that solid‐phase extraction combined with gas chromatography and quadrupole mass spectrometry data and partial least squares discriminant analysis provides a suitable tool to discriminate wines, both in terms of geographical origin as well as wine type and vintage. 相似文献
148.
QuEChERS sample preparation for the determination of pesticides and other organic residues in environmental matrices: a critical review 总被引:4,自引:0,他引:4
Maria Concetta Bruzzoniti Leonardo Checchini Rosa Maria De Carlo Serena Orlandini Luca Rivoira Massimo Del Bubba 《Analytical and bioanalytical chemistry》2014,406(17):4089-4116
Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) is an extraction and clean-up technique originally developed for recovering pesticide residues from fruits and vegetables. Since its introduction, and until December 2013, about 700 papers have been published using the QuEChERS technique, according to a literature overview carried out using SciFinder, Elsevier SciVerse, and Google search engines. Most of these papers were dedicated to pesticide multiresidue analysis in food matrices, and this topic has been thoroughly reviewed over recent years. The QuEChERS approach is now rapidly developing beyond its original field of application to analytes other than pesticides, and matrices other than food, such as biological fluids and non-edible plants, including Chinese medicinal plants. Recently, the QuEChERS concept has spread to environmental applications by analyzing not only pesticides but also other compounds of environmental concern in soil, sediments, and water. To the best of our knowledge, QuEChERS environmental applications have not been reviewed so far; therefore, in this contribution, after a general discussion on the evolution and changes of the original QuEChERS method, a critical survey of the literature regarding environmental applications of conventional and modified QuEChERS methodology is provided. The overall recoveries obtained with QuEChERS and other extraction approaches (e.g., accelerated solvent extraction, ultrasonic solvent extraction, liquid/solid extraction, and soxhlet extraction) were compared, providing evidence for QuEChERS higher recoveries for various classes of compounds, such as biopesticides, chloroalkanes, phenols, and perfluoroalkyl substances. The role of physicochemical properties of soil (i.e., clay and organic carbon content, as well as cation exchange capacity) and target analytes (i.e., log KOW, water solubility, and vapor pressure) were also evaluated in order to interpret recovery and matrix effect data. 相似文献
149.
Rosaria Cozzolino Laura De Magistris Paola Saggese Matteo Stocchero Antonella Martignetti Michele Di Stasio Antonio Malorni Rosa Marotta Floriana Boscaino Livia Malorni 《Analytical and bioanalytical chemistry》2014,406(19):4649-4662
Autism spectrum disorders (ASDs) are a group of neurodevelopmental disorders which have a severe life-long effect on behavior and social functioning, and which are associated with metabolic abnormalities. Their diagnosis is on the basis of behavioral and developmental signs usually detected before three years of age, and there is no reliable biological marker. The objective of this study was to establish the volatile urinary metabolomic profiles of 24 autistic children and 21 healthy children (control group) to investigate volatile organic compounds (VOCs) as potential biomarkers for ASDs. Solid-phase microextraction (SPME) using DVB/CAR/PDMS sorbent coupled with gas chromatography–mass spectrometry was used to obtain the metabolomic information patterns. Urine samples were analyzed under both acid and alkaline pH, to profile a range of urinary components with different physicochemical properties. Multivariate statistics techniques were applied to bioanalytical data to visualize clusters of cases and to detect the VOCs able to differentiate autistic patients from healthy children. In particular, orthogonal projections to latent structures discriminant analysis (OPLS-DA) achieved very good separation between autistic and control groups under both acidic and alkaline pH, identifying discriminating metabolites. Among these, 3-methyl-cyclopentanone, 3-methyl-butanal, 2-methyl-butanal, and hexane under acid conditions, and 2-methyl-pyrazine, 2,3-dimethyl-pyrazine, and isoxazolo under alkaline pH had statistically higher levels in urine samples from autistic children than from the control group. Further investigation with a higher number of patients should be performed to outline the metabolic origins of these variables, define a possible association with ASDs, and verify the usefulness of these variables for early-stage diagnosis. Figure
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150.
Rodrigues Ana Luísa Marques Rosa Dias Maria Isabel Prudêncio Maria Isabel Russo Dulce Diniz Mariana Martins Andrea Neves César Kasztovszky Zsolt Harsányi Ildiko Szilágyi Veronika Kovács Imre Szőkefalvi-Nagy Zoltán 《Journal of Radioanalytical and Nuclear Chemistry》2022,331(9):3887-3903
Journal of Radioanalytical and Nuclear Chemistry - A contribution to the discussion about Vila Nova de São Pedro (VNSP) as a production centre of symbolic lithic artefacts, the origin of raw... 相似文献