Surface modification of glassy carbon electrode with the functionalized carbon nanotube for ultrasensitive electrochemical detection of risperidone

Risperidone (RIS), one of the typical antipsychotics drugs, originally approved to be used for the mental illness treatment, especially schizophrenia, bipolar disorder, autism and major depression. In the present study, different carbon nanostructures including functionalized multi-walled carbon nanotubes (F-MWCNTs), carbon nanoparticles, nanodiamond-graphite and reduced graphene oxide were employed for modification of the surface of glassy carbon electrode (GCE) for ultrasensitive detection of RIS. The most significant increase in the anodic peak current of RIS was observed on F-MWCNTs-modified electrode (compared to the other modified electrodes and bare GCE). The influence of different experimental parameters such as pH of the buffered solutions, the amount of the modifier and time and potential of the accumulation was optimized by monitoring the LSV responses toward RIS for the selected modified electrode. A wide linear dynamic range of 0.04–7 µM with a low detection limit of 12 nM was obtained. The results exhibit an acceptable performance of the proposed electrode for determination of RIS in the pharmaceutical and clinical preparations.     

Synthesis of a polymer-capped palladium nanoparticles and its application as a reusable catalyst in oxidative coupling reaction of α-hydroxyketones and 1,2-diamines for preparation of pyrazines and quinoxalines

A novel method for the synthesis of pyrazines and quinoxalines has been developed using α-hydroxyketones and 1,2-diamines in the presence of cross-linked poly(4-vinylpyridine)-stabilized Pd(0) nanoparticles, [P4-VP]-PdNPs. The catalyst was easily prepared and characterized using various techniques such as FT-IR and UV–Vis spectroscopy, AAS, TEM, FESEM, EDX analysis and XRD. The results confirm a good dispersion of palladium nanoparticles on the polymer support. The catalyst displayed good catalytic activity when applied to the synthesis of quinoxalines via condensation of α-hydroxyketones with 1,2-diamines. A few pyrazine derivatives and various quinoxalines are prepared via coupling reaction of α-hydroxyketones and 1,2-diamines in high–excellent yields (81–99%) with short reaction times. The quinoxalines products were characterized by FT-IR, ¹H and ¹³C NMR spectroscopy, and the physical properties were compared to the literature values of known compounds. The advantages of the present method over conventional classical methods are rapid and very simple work-up, and the catalyst is reusable many times without a significant loss in its activity.     

N-Doped Hybrid Graphene and Boron Nitride Armchair Nanoribbons As Nonmagnetic Semiconductors with Widely Tunable Electronic Properties

Russian Journal of Physical Chemistry A - The electronic and chemical properties of N-doped hybrid graphene and boron nitride armchair nanoribbons (N-doped a-GBNNRs) in comparison with graphene...     

Design of a highly efficient and water-tolerant sulfonic acid nanoreactor based on tunable ordered porous silica for the von Pechmann reaction

Among a number of different sulfonic acid nanoreactors prepared, 5 having both acidic sites and phenyl groups located inside the mesochannels of SBA-15 was shown to be the most active and reusable catalyst in the von Pechmann reaction. The mesochannels, and covalently anchored organic groups, provide a synergistic means of an efficient approach of the reactants to acidic sites, enough space for the subsequent cyclization, and suitable hydrophobicity to drive out the water byproduct.     

Highly efficient synthesis of 3-pyrrolyl-indolinones and pyrrolyl-indeno[1,2-b]quinoxalines catalyzed by heteropolyacids

Simple and improved conditions have been found for the synthesis of 3-pyrrolyl-indolinones and pyrrolyl-indeno[1,2-b]quinoxalines by coupling of 4-hydroxyproline with isatins and 11H-indeno[1,2-b]quinoxalin-11-ones using Keggin (H₃PW₁₂O₄₀) and Well-Dawson tungsten heteropolyacids (H₆P₂W₁₈O₆₂).     

Solid phase extraction of copper (II) by sorption on octadecyl silica membrane disk modified with a new Schiff base and determination with atomic absorption spectrometry

A simple, selective and reliable method for rapid extraction and determination of trace amounts of Cu (II) ions from aqueous samples using octadecyl-bonded silica membrane disks modified with bis-(3-methoxy salicylaldehyde)-1,6-diaminohexane and flame atomic absorption spectrometry (FAAS) is presented. Extraction efficiency, the influence of pH, flow rates, amount of ligand, and type and least amount of eluant were investigated. The linear dynamic range of the proposed method for Cu (II) ions was found in a wide concentration range of 1.0 (± 0.2)–150 (± 2) μg l^− 1. The detection limit and preconcentration factor of this method were found 30.0 (± 0.7) ng l^− 1 and 100 respectively. The reproducibility of the procedure is at the most 2.0%. The effects of various cationic interferences on the percent recovery of copper ion were studied. The method was used to the recovery of copper ion from different synthetic, alloys and biological samples.     

Sorptive thin film microextraction followed by direct solid state spectrofluorimetry: A simple,rapid and sensitive method for determination of carvedilol in human plasma

A poly acrylate-ethylene glycol (PA-EG) thin film is introduced for the first time as a novel polar sorbent for sorptive extraction method coupled directly to solid-state spectrofluorimetry without the necessity of a desorption step. The structure, polarity, fluorescence property and extraction performance of the developed thin film were investigated systematically. Carvedilol was used as the model analyte to evaluate the proposed method. The entire procedure involved one-step extraction of carvedilol from plasma using PA-EG thin film sorptive phase without protein precipitation. Extraction variables were studied in order to establish the best experimental conditions. Optimum extraction conditions were the followings: stirring speed of 1000 rpm, pH of 6.8, extraction temperature of 60 °C, and extraction time of 60 min. Under optimal conditions, extraction of carvedilol was carried out in spiked human plasma; and the linear range of calibration curve was 15–300 ng mL⁻¹ with regression coefficient of 0.998. Limit of detection (LOD) for the method was 4.5 ng mL⁻¹. The intra- and inter-day accuracy and precision of the proposed method were evaluated in plasma sample spiked with three concentration levels of carvedilol; yielding a recovery of 91–112% and relative standard deviation of less than 8%, respectively. The established procedure was successfully applied for quantification of carvedilol in plasma sample of a volunteer patient. The developed PA-EG thin film sorptive phase followed by solid-state spectrofluorimetric method provides a simple, rapid and sensitive approach for the analysis of carvedilol in human plasma.     

Sensitive determination of iron(III) by gold electrode modified with 2-mercaptosuccinic acid self-assembled monolayer

Preparation and application of gold 2-mercaptosuccinic acid self-assembled monolayer (Au-MSA SAM) electrode for determination of iron(III) in the presence of iron(II) is described by cyclic voltammetry, electrochemical impedance spectroscopy, and Osteryoung square wave voltammetry. The square wave voltammograms showed a sharp peak around positive potentials +0.250 V that was used for construction of the calibration curve. Parameters influencing the method were optimized. A linear range calibration curve from 1.0 × 10⁻¹⁰ to 6.0 × 10⁻⁹ M iron(III) with a detection limit of 3.0 × 10⁻¹¹ M and relative standard deviation (R.S.D.) of 6.5% for n = 8 at 1.0 × 10⁻⁹ M iron(III) was observed in the best conditions. Possible interferences from the coexisting ions were also investigated. The results demonstrated that sensor could be used for determination of iron(III) in the presence of various ions. The validity of the method and applicability of the sensor were successfully tested by determining of iron(III) in natural waters (tap and mineral waters) and in a pharmaceutical sample (Venofer^® ampoule) without interference from sample matrix. The experimental data are presented and discussed from which the new sensor is characterized.     

Chemically modified multiwalled carbon nanotubes as efficient and selective sorbent for separation and preconcentration of trace amount of Co(II), Cd(II), Pb(II), and Pd(II)

Multi-walled carbon nanotubes (MWCNTs) were chemically functionalized by glutaric dihydrazide (GDH) and characterized with FT-IR technique. This new sorbent was used for enrichment and preconcentration of Co(II), Cd(II), Pb(II), and Pd(II) ions. The adsorption was achieved quantitatively on MWCNTs at pH 4.0, and then the retained metal ions on the adsorbent were eluted with 1.5 mol L^?1 HNO₃. The effects of analytical parameters including pH of the solution, eluent type, sample volume, and matrix ions were investigated for optimization of the presented procedure. The adsorption capacity of the adsorbent at optimum conditions was found to be 33.6, 29.2, 22.1, and 36.0 mg g^?1 for Co(II), Cd(II), Pb(II), and Pd(II), respectively. The LOD values of the method were 0.16, 0.19, 0.17, and 0.12 ng mL^?1 (3Sb, n = 10) for Co(II), Cd(II), Pb(II), and Pd(II), respectively. The RSDs values of the method were 0.75, 0.85, 1.16, and 1.30 ng mL^?1 for Co(II), Cd(II), Pb(II), and Pd(II), respectively. The method was applied for the determination of analytes in soil, well water, and wastewater samples with satisfactory results.     

Cavity shape effect on pKa prediction of small amines

Cavity shape affects the free energy of solvation by which pK_a changes. In this work, we have used different level of theories and basis sets combine with the PCM model of solvation to predict acidity constants of small ammonium ions during their protonation in aqueous solution. Three different kinds of models including UAHF, Bondi, and Pauling have been chosen to study that how a cavity shape changes acidity constant. Contrary to the previous results of literature for bulky ammonium ions, the difference between our results is not very much. Predictions show that in some levels and basis sets UAHF model is the best, while in some other cases it is the worst.