A novel strategy to increase performance of solid‐phase microextraction fibers: Electrodeposition of sol‐gel films on highly porous substrate

In the present work, the effect of substrate porosity for preparation of solid‐phase microextraction (SPME) fibers was investigated. The fibers were prepared by electrodeposition of sol‐gel coatings using negative potentials on porous Cu wire and compared with previous reported technique for preparation of SPME fibers using positive potentials on smooth gold wire. Porous substrate was prepared by electrodeposition of a thin layer of Cu on a Cu wire. The extraction capability of prepared fibers was evaluated through extraction of some aromatic hydrocarbons from the headspace of aqueous samples. The effect of substrate porosity and some operating parameters on extraction efficiency was optimized. The results showed that extraction efficiency of SPME fibers highly depends on porosity of the substrate. The LOD ranged from 0.005 to 0.010 ng/mL and repeatability at the 1 ng/mL was below 12%. Electrodeposited films were characterized for their surface morphology and thermal stability using SEM and thermogravimetric analysis, respectively. SEM analysis revealed formation of porous substrate and subsequently porous coating on the wire surface and thermogravimetric analysis showed high thermal stability of the prepared fiber.     

A green one-pot synthesis of N-alkyl-2-(2-oxoazepan-1-yl)-2-arylacetamide derivatives via an Ugi four-center,three-component reaction in water

This work describes a green and efficient one-pot synthesis of N-alkyl-2-(2-oxoazepan-1-yl)-2-arylacetamide derivatives via an Ugi four-center, three-component reaction of 6-aminohexanoic acid, aromatic aldehydes, and isocyanide derivatives in water under reflux conditions in the absence of a catalyst.     

A new look at XRD patterns of archaeological ceramic bodies

In this paper, the general rules of phase transformations in calcareous clay bodies during firing were used to estimate the equivalent firing temperature (EFT) of seventeenth century polychrome Persian haft rang tiles based on their X-ray diffraction (XRD) patterns. The novelty of this work is, however, that it handles the XRD patterns of archaeological clay bodies with principal component analysis (PCA) in order to have a new look at their firing and thermal behaviour. Statistically handling the XRD patterns, different clusters were discriminated in the clay bodies whose mineralogical composition showed various proportions of amorphous and quartz contents. The results showed interesting trends in the different clusters in terms of the EFT, quartz content and the density of the bodies. The present work uses PCA to have a new look at XRD patterns of archaeological clay bodies and, moreover, to interpret the PCA results in order to estimate the EFT of a large number of archaeological clay bodies.     

Polyvinylimidazole/sol–gel composite as a novel solid‐phase microextraction coating for the determination of halogenated benzenes from aqueous solutions

A polyvinylimidazole/sol–gel composite is proposed as a novel solid‐phase microextraction fiber to extract five halobenzenes from the headspace of aqueous solutions in combination with gas chromatography with mass spectrometry. The prepared fiber was characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. The obtained results showed that porous polyvinylimidazole/sol–gel composite was chemically deposited on fused silica fiber. The effect of important extraction parameters including extraction temperature, extraction time, and salt content were investigated. The optimum conditions were as follows: extraction temperature 25°C, extraction time 20 min, and salt concentration 30 w/v%. Detection limits and relative standard deviations of the developed method for halogenated benzenes were below 0.1 pg/mL and 15%, respectively. Repeatability of the proposed method, explained by relative standard deviation, varied between 5.48 and 9.15% (n = 5). The limits of detection (S/N = 3) ranged between 0.01 and 0.10 ng/L using gas chromatography with mass spectrometry with selected ion monitoring mode. For real sample analysis, three types of water samples with different matrices (ground, surface, and tap water) were studied. The optimized procedure was applied to extraction and method validation of halogenated benzenes in spiked water samples.     

Synthesis of Arylidene – Isoquinolinones bearing Combretastatin Skeleton by Cyclocarbopalladation/cross coupling Tandem Heck-Suzuki Miaura Reactions using nano catalyst Pd@Py-IL-SPION

Cyclocarbopalladation/cross-coupling cascade intramolecular Heck–Suzuki–Miyaura reactions is applied for the first time by palladium immobilized on pyridine-imidazolium ionic liquid supported magnetic iron oxide nanoparticle catalyst (denoted Pd@Py-IL-SPION) for the last step to synthesize trisubstituted arylidene–isoquinolinones derivatives having Combretastatin skeleton. The reaction is performed via propargylamide intermediates prepared by Ugi 4-CR reactions, which undergoes intramolecular Heck–Suzuki–Miyaura domino reaction to produce the desired trisubstituted arylidene-isoquinolinones. The method shows full regio- and stereoselectivity derives from the particular Pd-catalyzed syn-insertion of triple bond.     

Computational studies on the conformational preference of N-(Thiazol-2-yl) benzamide

N-(Thiazol-2-yl) benzamide 1 substructures are found in some of bioactive compounds. In some of protein/ligand co-crystals, the 1 moiety adopts a conformer in which the amide O and the thiazole S atoms are close. In fact, in the crystalline structure of 1 , the O—S distance is even shorter than Van der Waals radius. Although the natural bond orbital analysis finds a weak stabilizing interaction between O and S atoms, the attractive dipole–dipole interaction between the amide N─H and thiazole N atom seems to play a more significant role. Moreover, an intramolecular O—H hydrogen bonding in dimeric forms found to have an important role in the conformation preference of 1 . Computational details for the stability of conformers have been discussed using quantum theory of atoms in molecules, natural bond orbital (NBO) and noncovalent interaction index analysis.     

ZnO/Fe3O4 nanoparticles promoted green synthesis of pyrazolo pyrimidinones: Study of antioxidant activity

The preparation of pyrazolo pyrimidinone derivatives was performed by using five component reactions of phthalaldehyde, cyanomethylamine, electron deficient acetylenic compounds, isocyanate, hydrazine, and catalytic amounts of ZnO/Fe₃O₄-magnetic nanoparticles as a high performance catalyst under ultrasonic conditions at ambient temperature in aquause media at room temperature. It should be mentioned that this catalyst was prepared using Spinacia oleracea water extract. In addition, for investigation of antioxidant ability, radical trapping by DPPH and reducing power of ferric ion experiments was performed. As a result, synthesized compounds show excellent radical trapping by DPPH and good reducing ability of ferric ion. The current procedure has the benefits for instance excellent yield of reaction, green media, and easy separation of product and catalyst.     

Monitoring of Anti Cancer Drug Letrozole by Fast Fourier Transform Continuous Cyclic Voltammetry at Gold Microelectrode

A continuous cyclic voltammetric study of letrozole at gold microelectrode was carried out. The drug in phosphate buffer (pH 2.0) is adsorbed at ?200 mV, giving rise to change in the current of well‐defined oxidation peak of gold in the flow injection system. The proposed detection method has some of advantages, the greatest of which are as follows: first, it is no more necessary to remove oxygen from the analyte solution and second, this is a very fast and appropriate technique for determination of the drug compound in a wide variety of chromatographic analysis methods. Signal‐to‐noise ratio has significantly increased by application of discrete Fast Fourier Transform (FFT) method, background subtraction and two‐dimensional integration of the electrode response over a selected potential range and time window. Also in this work some parameters such as sweep rate, eluent pH, and accumulation time and potential were optimized. The linear concentration range was of 1.0×10^?7?1.0×10^?10 mol/L (r=0.9975) with a limit of detection and quantitation 0.08 nmol/L and 0.15 nmol/L, respectively. The method has the requisite accuracy, sensitivity, precision and selectivity to assay letrozol in tablets. The influences of pH of eluent, accumulation potential, sweep rate, and accumulation time on the determination of the letrozol were considered.     

Highly selective fluorescent recognition of Zn2+ based on naphthalene macrocyclic derivative

A new macrocyclic chemosensor containing two naphthalene fluorophores has been synthesized. The fluorescent properties of this receptor has been studied in the presence of various metal ions such as Na⁺, Ag⁺, Cr³⁺, Mn²⁺, Fe³⁺, Co²⁺, Ni²⁺, Cu²⁺, Zn²⁺, Cd²⁺ and Pb²⁺. When increasing concentrations of Zn²⁺ ions were introduced, the emission of L was drastically increased (EFE = 4.34). This special change was not observed when other metal ions were used; such highly selective fluorescent response indicates that this receptor can easily discriminate Zn²⁺ ions from other similar species. Model calculations at DFT level further suggest the possible interaction mode, and relatively steric position between the host and guest also influence the optical response.     

Biosurfactant production under extreme environmental conditions by an efficient microbial consortium, ERCPPI-2

The biosurfactant production potential of a new microbial consortium of Enterobacter cloacae and Pseudomonas sp. (ERCPPI-2) which was isolated from heavy crude oil-contaminated soil in the south of Iran, has been investigated under extreme environmental conditions. The isolated consortium produces a biosurfactant mixture with excessive oil spreading and emulsification properties. This consortium was able to grow and produce biosurfactant at temperatures up to 70 °C, pressures up to 6000 psia, salinities up to 15% (w/v), and in the pH range 4-10. Besides, the optimum biosurfactant production conditions were found to be 40 °C and 7.0 for the temperature and pH value, respectively. These conditions gave the best biosurfactant production of 1.74 g/1 when the cells were grown on a minimal salt medium containing 1.0% (w/v) olive oil, 1.0% (w/v) sodium nitrate supplemented with 1.39% (w/v) K(2)HPO(4) at 40 °C and 150 rpm after 48 h of incubation. The ERCPPI-2 could reduce surface and interfacial tensions to 31.7 and 0.65 mN/m from the original values of 58.3 and 16.9 mN/m, respectively. The isolated consortium produced biosurfactant using heavy crude oil as the sole source of carbon and emulsified the available heavy crude oil up to E(24)=83.4%. The results of the core holder flooding tests at simulated reservoir conditions demonstrated that the oil recovery efficiency due to the injection of the cell-free biosurfactant solution was 27.2%, and the bacterium injection reduced the final residual oil saturations to below 3% at optimum conditions.