Picolinimidoamide-Cu(II) complex anchored on Fe3O4@SiO2 core–shell magnetic nanoparticles: an efficient reusable catalyst for click reaction

A Cu(II) complex supported on Fe₃O₄@SiO₂ core–shell magnetic nanoparticles (MNPs) was prepared and characterized by FT-IR, XRD, SEM, EDX, TEM, VSM, TGA, and AAS analysis. The load of Cu on picolinimidoamide ligand anchored on Fe₃O₄@SiO₂ core–shell MNPs was determined as 1.22, 1.54, and 1.70 wt% using AAS, EDX and TGA analyses, respectively. Synthesized Cu(II) complex on Fe₃O₄@SiO₂ MNPs efficiently catalyzed a click reaction between alkyl halides, alkynes, and sodium azide to synthesize corresponding triazoles in high to excellent yields. The catalyst was recovered using an external magnetic field, and recycled for subsequent reactions without substantial loss of efficiency.     

Gas chromatographic separation of optically active anti-inflammatory 2-arylpropionic acids using (+)- or (-)-amphetamine as derivatizing reagent

A method is described for the derivatization of several non-steroidal anti-inflammatory arylalkanoic acids (ibuprofen, ketoprofen, naproxen, fenoprofen, flurbiprofen, pirprofen, cicloprofen, tiaprofenic acid, etodolic acid) with optically active amphetamine. The usefulness of this reagent compared to alpha-methylbenzylamine is described. The enantiomers are separated as diastereoisomers using capillary gas chromatography with nitrogen-phosphorus detection. The procedure is readily applied to the quantification of the enantiomers in urine and plasma samples.     

Stereospecific high-performance liquid chromatographic assay of pirprofen enantiomers in rat plasma and urine.

A stereospecific high-performance liquid chromatographic method was developed for the assay of pirprofen enantiomers in rat plasma and urine. Following addition of internal standard (ketoprofen) and acidifier (L-ascorbic acid) to biological fluids, pirprofen was extracted into an isopropanol-isooctane (5:95) mixture. Diastereomers of pirprofen enantiomers, which were formed using L-leucinamide, were separated on a reversed-phase column with ultraviolet detection at 275 nm using 0.06 M KH2PO4-acetonitrile-triethylamine (64:36:0.1) as mobile phase. The limit of quantitation was 0.1 microgram/ml for each enantiomer, based on 100 microliters of rat plasma. No spontaneous oxidation of pirprofen to its pyrrole metabolite occurred during sample preparation and analysis. In three female rats which were dosed with 10 mg/kg racemic pirprofen orally, plasma concentrations of the enantiomers could be followed for 24 h. Pirprofen enantiomers in plasma were virtually unconjugated, and negligible concentrations of pyrrole metabolites were observed. Less than 10% of the total dose was recovered in urine as intact drug and its glucuroconjugates. The assay was found suitable for the study of the pharmacokinetics of pirprofen enantiomers in the rat.     

Antireflection properties of germanium–carbon coating on zinc supplied substrate

In this research, germanium–carbon coatings were deposited on ZnS and glass substrates by a RF plasma enhanced chemical vapor deposition method using GeH₄ and CH₄ as precursors. ZnS/Ge_1?xC_x double-layer antireflection coating with optical thickness of one quarter wavelength was designed. The samples were characterized by fourier transform infrared spectroscopy, X-ray diffraction (XRD), field emission scanning electron microscopy and nanoindentation. The coatings exhibited a structure free of pores with a very good adhesion to substrate. Based on the XRD patterns, no diffraction peak was found, so all the coatings mainly had an amorphous structure. The infrared (IR) transmittance spectrum show that the maximum IR transmittance in the band of 1030–1330 cm^?1 was about 84.6%, which is higher than ZnS substrate by 10%. In addition, the reflection of ZnS substrate is about 25%. This system has reduced the reflection from the substrate by 15%.     

Determination of Toxic Elements in Muscle Tissues of Five Fish Species Using Ultrasound‐Assisted Pseudodigestion by Electrothermal Atomic Absorption Spectrophotometry: Optimization Study

A simple and rapid method is described for the determination of As, Cd, and Pb in muscle tissue of five freshwater fish species by ultrasound‐assisted pseudodigestion (USD). A Plackett‐Burman experimental design was used as a multivariate strategy for the evaluation of the effects of varying several variables at once. The variables such as sonication time (ST), sample mass of muscle tissues (SM), temperature of ultrasonic bath (T), nitric acid (A1), and mixture of acid and oxidant (A2) have been studied. From these studies, some variables showed significant effect on % recovery, and they were further optimized by a 2³+star central composite design, which involved 16 experiments. Optimum values of the variables were selected for the development of USD to determine the contents of As, Cd, and Pb in muscle tissue of five fish species, used as bioindicators for Lake Manchar (Sindh, Pakistan) to know whether consumption of these fishes threatens human health. The determination of three toxic elements under study was carried out by electrothermal atomic absorption spectrometry (ETAAS). The accuracy of the optimized procedure was evaluated by analysis of certified reference materials DORM‐2 (Dogfish Muscle Certified Reference Material for Trace Elements) and by comparison with conventional wet acid digestion methodology. No significant differences were observed for p=0.05 when comparing the values obtained by the proposed USD method and conventional digestion method (CDM) (paired t‐test). The average relative standard deviation of the USD method varied between 4.05%, 7.53%, and 4.55% for As, Cd, and Pb, respectively (n=10).     

Application of Polytyramine Nanoparticles to the Corrosion Protection of Copper

Electrochemical polymerization of tyramine was achieved on copper electrode surface from tyramine in 0.3 M oxalic acid (pH=1.2) solution by using cyclic voltammetry technique. The formation of polytyramine nanoparicles (PTN) were characterized by cyclic voltammetry (CV), fourier transform infrared‐attenuated total reflectance (FTIR‐ATR) spectroscopy and scanning electron microscopy (SEM). The corrosion behavior of PTN coated copper was investigated by means of the change of open circuit potential with exposure time (E_ocp t), electrochemical impedance spectroscopy (EIS) and anodic polarization curves in 3.5 % NaCl solutions at room temperature. The obtained results showed the shift of corrosion potential toward positive values for electropolymerized copper and a significant decrease in corrosion current and corrosion rate in comparison with bare copper, so that the PTNs coating could be used as an important protection against corrosion of copper.