4-(4′-Diamino-di-phenyl)-sulfone supported on hollow magnetic mesoporous Fe3O4@SiO2 NPs: As a reusable and efficient catalyst for the synthesis of ethyl 2-amino-5,10-dihydro-5,10-dioxo-4-phenyl-4H benzo[g]chromene-3-carboxylates

4-(4′-diamino-di-phenyl)-sulfone supported on hollow magnetic mesoporous (HMMS) Fe₃O₄@SiO₂ NPs has been used as a novel and efficient catalyst in the preparation of ethyl 2-amino-5,10-dihydro-5,10-dioxo-4-phenyl-4H benzo[g]chromene-3-carboxylates by a simple one-pot three-component reaction of aldehydes, ethyl cyanoacetate and 2-hydroxynaphthalene-1,4-dione under reflux conditions in ethanol. Wide range of products, excellent yields in short times, reusability of the catalyst, low catalyst loading and environmental benignity are some of the important features of this protocol.     

Development of a Reversed-Phase Liquid Chromatographic Assay for the Quantification of Total Persipeptides in Fermentation Broth

The emergence and prevalence of multi-drug-resistant bacterial strains increase the potential for outbreaks of incurable infections. The discovery of novel antibiotics and pharmacological preparations requires the identification of novel bioactive small molecules. A specific, sensitive, and reliable quantification method using high-performance liquid chromatography (HPLC) with UV detection was developed for the determination of total persipeptides (A and B), which are cyclic pentapeptides found in the fermentation broth of Streptomyces zagrosensis UTMC 1154 that exhibit bioactivity against methicillin-resistant Staphylococcus aureus (MRSA). A simple liquid–liquid extraction (LLE) method using butanol was employed to extract persipeptides from the fermentation broth prior to HPLC analysis. The chromatographic separation of persipeptides and the internal standard, virginiamycin, was achieved with a gradient of acetonitrile and water on a C18 reversed-phase analytical column in a 25-min analytical run utilizing a flow rate of 0.8 mL min⁻¹ and detection at 210 nm. The whole assay was validated, and the method presented a linear response range with a regression coefficient of determination R ² of 0.9996 for the quantification of persipeptides in the concentration range of 3.9–250.0 µg mL⁻¹, as well as extraction recoveries ranging from 54.78 ± 9.83 % to 56.45 ± 16.33 %. The bias and the precision of the proposed method were <10 %. The detection and quantification limits for the persipeptides were 27 and 83 µg L⁻¹, respectively.

     

Automated hollow‐fiber liquid‐phase microextraction followed by liquid chromatography with mass spectrometry for the determination of benzodiazepine drugs in biological samples

In this study, two‐phase hollow‐fiber liquid‐phase microextraction and three‐phase hollow‐fiber liquid‐phase microextraction based on two immiscible organic solvents were compared for extraction of oxazepam and Lorazepam. Separations were performed on a liquid chromatography with mass spectrometry instrument. Under optimal conditions, three‐phase hollow‐fiber liquid‐phase microextraction based on two immiscible organic solvents has a better extraction efficiency. In a urine sample, for three‐phase hollow fiber liquid‐phase microextraction based on two immiscible organic solvents, the calibration curves were found to be linear in the range of 0.6–200 and 0.9–200 μg L^?1 and the limits of detection were 0.2 and 0.3 μg L^?1 for oxazepam and lorazepam, respectively. For two‐phase hollow fiber liquid‐phase microextraction, the calibration curves were found to be linear in the range of 1–200 and 1.5–200 μg L^?1 and the limits of detection were 0.3 and 0.5 μg L^?1 for oxazepam and lorazepam, respectively. In a urine sample, for three‐phase hollow‐fiber‐based liquid‐phase microextraction based on two immiscible organic solvents, relative standard deviations in the range of 4.2–4.5% and preconcentration factors in the range of 70–180 were obtained for oxazepam and lorazepam, respectively. Also for the two‐phase hollow‐fiber liquid‐phase microextraction, preconcentration factors in the range of 101–257 were obtained for oxazepam and lorazepam, respectively.     

Density functional theory study of the regio‐ and stereoselectivity of 1,3-dipolar cycloaddition reactions between 2-ethylthio-4-phenyl-1-azetin and some substituted nitrile oxides

The mechanism (regio- and stereoselectivity) of 1,3-dipolar cycloaddition (1,3-DC) of 2-ethylthio-4-phenyl-1-azetin 1 with benzonitrile oxide 2a, 2-aminobenzonitrile oxide 2b and 2-azidobenzonitrile oxide 2c has been investigated by density functional theory-based reactivity indices and activation energy calculations at B3LYP/6-31G(d,p) level of theory in the gas and solvent phase. Thermodynamic and kinetic parameters of the possible ortho/meta regioisomeric and endo/exo stereoisomeric pathways have been determined. In order to rationalize complete endo selective fashion provided by these 1,3-DC cycloadditions, a natural steric analysis between NLMOs i,j for TS1ox and TS1on and also a second-order interaction energy, E ², analysis between the donor–acceptor orbitals in these TSs were carried out. In all cases, the ortho pathways are more favorable compared to the meta alternatives and it is found that the endo pathway is preferred. Our results show that these cycloadditions follow an asynchronous one-step mechanism with a nonpolar character. Theoretical data are in good agreement with the experimental results.     

Dispersion-corrected DFT study on the carbon monoxide sensing by B<Subscript>2</Subscript>C nanotubes: effects of dopant and interferences

Electrical sensitivity of a boron carbon nanotube (B₂CNT) was examined toward carbon monoxide (CO) molecule by using dispersion-corrected density functional theory calculations. It was found that CO is weakly adsorbed on the tube, releasing energy of 3.5–4.1 kcal/mol, and electronic properties of the tube are not significantly changed. To overcome this problem, boron and carbon atoms of the tube were substituted by aluminum and silicon atoms, respectively. Although both Al and Si doping make the tube more reactive and sensitive to CO, Si doping seems to be a better strategy to manufacture CO chemical sensors due to the higher sensitivity without deformation of nanotube structure after adsorption procedure. Moreover, it was shown that some interference molecules such as H₂O, H₂S and NH₃ cannot significantly change the electronic properties of B₂CNT. Therefore, the Si-doped tube might convert the presence of CO molecules to electrical signal.     

Convergence Theorems for Pointwise Asymptotically Strict Pseudo-Contractions in Hilbert Spaces

A new class of contractive mappings called pointwise asymptotically ?-strict pseudo-contractions in Hilbert spaces is introduced and weak convergence of the sequence generated by Mann's iterative scheme to a fixed point of a uniformly Lipschitzian and pointwise asymptotically ?-strict pseudo-contractive mapping T in a Hilbert space is established. Also, a new kind of monotone hybrid method which is a modification of Mann's iterative scheme for finding a common fixed point of an infinitely countable family of uniformly Lipschitzian and pointwise asymptotically ?-strict pseudo-contractive mappings is proposed. Strong convergence of the sequence generated by the proposedmonotone hybrid method for an infinitely countable family of uniformly Lipschitzian and pointwise asymptotically ?-strict pseudo-contractive mappings in a Hilbert space is also shown. The results presented in this article extend and improve some known results in the literature.     

Chiral separation of three agrochemical toxins enantiomers by high-performance liquid chromatography on a vancomycin crystalline degradation products-chiral stationary phase

This work aims to evaluate for the enantiomeric separations of three agrochemical toxins: haloxyfop-methyl, fenoxaprop-p-ethyl and indoxacarb on crystalline degradation products-chiral stationary phase (CDP-CSP) of high-performance liquid chromatography (HPLC) under normal and polar organic phases. In the normal phase, the mobile phase was n-hexane with alcohols including methanol and isopropanol as polar modifiers. In the polar organic phase mode, the mobile phase was methanol with different percentages of triethylammunium acetate. The influence of flow rate (0.3-0.9 mL/min), analyte concentration and silica gel particle sizes (10, 15 and 30 microm) was investigated. This new chiral stationary phase showed excellent stereoselectivity for the two enantiomers of haloxyfop-methyl and fenoxaprop-p-ethyl and chiral recognition for indoxacarb under normal-phase mode. However, under polar organic phase, only indoxacarb was separated (alpha < 1.5). The chromatographic results were compared with commercial chiral columns.     

Distances entre exponentielles et puissances d’éléments de certaines algèbres de Banach

Let A be a Banach algebra which does not contain any nonzero idempotent element, let γ > 0, and let . We show that if then . We also show, assuming a suitable spectral condition on x, that if , then Received: 12 July 2006 Revised: 31 January 2007     

The Minimal Cqupling of Charged spin-3/2 Fields to an Extended Abelian Gauge Model

Charged spin-3/2 fields are coupled to an extended gauge model without the total suppression of the vector degrees of freedom which usually takes place as a consequence of simultaneously imposing the Maxwell and Rarita-Schwinger U(1) symmetries.     

l‐Proline‐functionalized Fe3O4 nanoparticles as a novel magnetic chiral catalyst for the direct asymmetric Mannich reaction

l ‐Proline has been successfully anchored on the surface of magnetic nanoparticles and characterized using powder X‐ray diffraction, scanning electron microscopy, vibrating sample magnetometry and Fourier transform infrared spectroscopy. These nanoparticles as a chiral catalyst have been employed to promote the direct asymmetric Mannich reaction. The corresponding products are obtained in high yields with high level of diastereoselectivity (up to 99:1 dr) in the presence of Fe₃O₄– l ‐proline. Also this heterogeneous catalyst can be recovered easily and reused many times without significant loss of its catalytic activity. Copyright © 2015 John Wiley & Sons, Ltd.