Stability‐indicating HPTLC method for quantitative estimation of silybin in bulk drug and pharmaceutical dosage form

In the present study a novel stability‐indicating high‐performance thin‐layer chromatography (HPTLC) method for quantitative determination of silybin in bulk drug and nanoemulsion formulation has been developed and validated on silica using solvent chloroform–acetone–formic acid (9 : 2 : 1 v/v/v) (R_f of silybin 0.46 ± 0.05) in the absorbance mode at 296 nm. The method showed a good linear relationship (r² ± 0.999) in the concentration range 25–1500 ng per spot. It was found to be linear, accurate, precise, specific, robust and stability‐indicating and can be applied for quality control and standardization of several multi‐component hepatoprotective formulations as well as for stability testing of different dosage forms. The method proposed was also used to investigate the kinetics of acidic and alkaline degradation processes by quantification of drug at different temperature to calculate the activation energy and half‐life for silymarin degradation. Copyright © 2009 John Wiley & Sons, Ltd     

Quantitative estimation of riluzole in human plasma by LC-ESI-MS/MS and its application to a bioequivalence study

A novel simple, sensitive, selective, and rapid high-performance liquid chromatography coupled with tandem mass spectrometry method was developed and validated for quantification of riluzole in human plasma. The chromatography was performed by using a Zorbax-SB-C18 (4.6 × 75 mm, 3.5 μm) column , isocratic mobile phase 0.1% formic acid/acetonitrile (10:90 v/v), and an isotope-labeled internal standard (IS), [¹³C,¹⁵N₂]riluzole. The extraction of drug and internal standard was performed by liquid–liquid extraction and analyzed by MS in the multiple reaction monitoring (MRM) mode using the respective [M+H]⁺ ions, m/z 235.0/165.9 for riluzole and m/z 238.1/169.0 for the IS. The calibration curve was linear over the concentration range 0.5–500.0 ng/ml for riluzole in human plasma. The limit of quantification (LOQ) was demonstrated at 0.5 ng/ml. The within-batch and between-batch precision were 0.6–2.3% and 1.4–5.7%, and accuracy was 97.1–101.1% and 98.8–101.2% for riluzole respectively. Drug and IS were eluted within 3.0 min. The validated method was successfully applied in a bioequivalence study of riluzole in human plasma.     

Cell Disruption Optimization and Covalent Immobilization of β-D-Galactosidase from <Emphasis Type="Italic">Kluyveromyces marxianus</Emphasis> YW-1 for Lactose Hydrolysis in Milk

β-D-galactosidase (EC 3.2.1.23) from Kluyveromyces marxianus YW-1, an isolate from whey, has been studied in terms of cell disruption to liberate the useful enzyme. The enzyme produced in a bioreactor on a wheat bran medium has been successfully immobilized with a view to developing a commercially usable technology for lactose hydrolysis in the food industry. Three chemical and three physical methods of cell disruption were tested and a method of grinding with river sand was found to give highest enzyme activity (720 U). The enzyme was covalently immobilized on gelatin. Immobilized enzyme had optimum pH and temperature of 7.0 and 40 °C, respectively and was found to give 49% hydrolysis of lactose in milk after 4 h of incubation. The immobilized enzyme was used for eight hydrolysis batches without appreciable loss in activity. The retention of high catalytic activity compared with the losses experienced with several previously reported immobilized versions of the enzyme is significant. The method of immobilization is simple, effective, and can be used for the immobilization of other enzymes.     

Synthesis,characterization, dielectric and rectification properties of PANI/Nd2O3:Al2O3 nanocomposites

Polyaniline–Nd₂O₃:Al₂O₃ nanocomposites were prepared by in situ oxidative polymerization method using different weight percentages of oxide powders. The prepared nanocomposites were characterized by Fourier transform infrared spectroscopy and X‐ray diffraction for molecular and crystal structures. Scanning electron microscopy and transmission electron microscopy images show the tubular structure of polyaniline nanocomposite with embedded metal oxides. The electrical conductivity of the nanocomposites increases with increase in temperature as well as with concentration of Nd₂O₃:Al₂O₃ particles in polyaniline. This is because of the hopping of charge polarons and extended chain length of the nanocomposites as evidenced by the negative thermal coefficient (NTC) characteristic. A high NTC value of 2.67 was found in nanocomposites with 15 wt% of oxide particles. These nanocomposites show low dielectric constant and dielectric loss; the electrical conductivity is higher than 0.3 S/cm as confirmed by Cole–Cole plot that indicates a decrease in both grain resistance and bulk resistance of the nanocomposites. The current–voltage and capacitance–voltage measurements were also carried out. The carrier mobility μ values of pure polyaniline and nanocomposites were found to be 4.27 × 10^?3 and 1.45 × 10^–2 H.M^?1, respectively. A significant enhancement in carrier mobility was observed in comparison with the literature. Copyright © 2016 John Wiley & Sons, Ltd.     

CuI mediated synthesis of heterocyclic flavone-benzofuran fused derivatives

An efficient synthetic method of heterocyclic flavone benzofuran fused derivatives is reported in good to excellent yield (75–90%) via Ullmann type coupling reaction. The protocol involves catalytic amount of CuI (10 mol%) and K₂CO₃ base for the intramolecular CO bond formation under mild reaction conditions.     

Simple and rapid synthesis of ternary polyaniline/titanium oxide/graphene by simultaneous TiO<Subscript>2</Subscript> generation and aniline oxidation as hybrid materials for supercapacitor applications

This paper reports a simple methodology for the synthesis of a polyaniline/titanium oxide/graphene hybrid (Pani/TiO₂/GN) using a simple methodology, and their application as a supercapacitor electrode material for energy storage. The Pani/TiO₂/GN hybrid was prepared by a simple approach by simultaneous generation of Pani and TiO₂ in situ from aniline and titanium iso-propoxide, respectively, in the presence of GN under ice bath conditions. The incorporation of GN improved the electrical conductivity of Pani and helped to decrease the charge transfer resistance, whereas TiO₂ generation by an in situ method increased the surface area considerably and enhanced the capacitance of the Pani/TiO₂/GN hybrid. TEM showed that Pani and TiO₂ were well incorporated and coated on the GN successfully. The shift of the peaks in the FTIR spectrum and XRD pattern of the Pani/TiO₂/GN hybrid compared to their pure counterparts suggested that TiO₂ and Pani had been perfectly coated on the GN, and there was a strong interaction among Pani, GN, and TiO₂ particles. The electrochemical performance of the as-prepared Pani/TiO₂/GN hybrid electrode showed a high specific capacitance of 403.2 F g^?1 at a current density of 2 A g^?1 and excellent cycling stability for up to 1000 cycles. This suggested that the effective incorporation of GN and TiO₂ into Pani and the high surface area could simultaneously increase the electrochemical capacitance and cyclic stability of the Pani/TiO₂/GN hybrid, leading to superior electrochemical performance.

Open image in new window

Graphical abstract The electrochemical performance of as-prepared Pani/TiO₂/GN hybrid electrode showed a high specific capacitance of 403.2 F g^?-1 at a current density of 2 A g^?-1 and excellent cycling stability for up to 1000 cycles. This suggested that the effective incorporation of GN and TiO₂ into Pani and the high surface area could simultaneously increase the electrochemical capacitance and cycle stability of the Pani/TiO₂/GN hybrid, leading to superior electrochemical performance.

     

Synthesis and Coordination Behavior of a New Hybrid Bidentate Ligand with Phosphine and Silylene Donors

This work describes the synthesis and coordination behavior of a new mixed-donor ligand PhC(NtBu)₂SiC₆H₄PPh₂ ( 1 ) containing both silylene and phosphine donor sites. Ligand 1 was synthesized from a reaction of ortho-lithiated diphenylphosphinobenzene (LiC₆H₄PPh₂) with chlorosilylene (PhC(NtBu)₂SiCl). Treatment of 1 with Se and GeCl₂ resulted in Si^IV compounds 2 and 3 by selective oxidation of the silylene donor. This strong σ-donor ligand induces dissociation of CuCl and PhBCl₂ leading to formation of ionic complexes 4 and 5 respectively. The reaction of 1 with ZnCl₂ and AlCl₃ resulted in the formation of chelate complexes 5 and 7 , respectively, while treatment with EtAlCl₂ and GaCl₃ forms monodentate complexes 8 and 9 . X-ray analysis of 4 showed that the copper is in the spiro center of the two five-membered rings. Moreover, the copper(I)chloride has not been oxidized but dissociates to Cu⁺ and [CuCl₂]⁻. All the compounds are well characterized by mass spectrometry, elemental analysis, NMR spectroscopy, and single-crystal X-ray diffraction studies.     

Generalizations of the area theorem for meromorphic univalent functions with nonzero pole

In this article, we consider meromorphic univalent functions f in the unit disc of the complex plane having a simple pole at z = α ∈ (0, 1) with nonzero residue b at z = α. In 1969, P.N. Chichra proved an area theorem for such functions. In this note, we generalize this theorem and prove an interesting consequence of this result.     

Performance evaluation of praseodymium doped fiber amplifiers

Optical Review - In this paper, we report the performance evaluation of praseodymium doped fiber amplifier (PDFA) operating in 1.25–1.35&nbsp;μm band of wavelengths based on...     

Immobilization of tris(1,10-phenanthroline)ruthenium with graphene oxide for electrochemiluminescent analysis

Electrochemiluminescence (ECL) of ruthenium complexes has broad applications and the immobilization of Ru(bpy)₃²⁺ has received extensive attention. In comparison with Ru(bpy)₃²⁺, Ru(phen)₃²⁺ can be immobilized more easily because of its better adsorbability. In this study, immobilization of Ru(phen)₃²⁺ for ECL analysis has been demonstrated for the first time by using graphene oxide (GO) as an immobilization matrix. The immobilization of Ru(phen)₃²⁺ is achieved easily by mixing Ru(phen)₃²⁺ with GO without using any ion exchange polymer or covalent method. The strong binding of Ru(phen)₃²⁺ with GO is attributed to both the π–π stacking interaction and the electrostatic interaction. The Ru(phen)₃²⁺/GO modified electrode was characterized by using tripropylamine (TPA) as the coreactant. The linear range of TPA is from 3 × 10⁻⁷ to 3 × 10⁻² mol L⁻¹ with the detection limit of 3 × 10⁻⁷ mol L⁻¹. The ECL sensor demonstrates outstanding long-term stability. After the storage in the ambient environment for 90 days, the ECL response remains comparable with its original signal.