Development and validation of a micellar high-performance liquid chromatographic method for determination of risedronate in raw material and in a pharmaceutical formulation: application to stability studies

A micellar HPLC method was developed for analysis of the antiosteoporosis drug risedronate. The analysis was carried out using a 250 x 4.6 mm id, 5 microm particle size C18 Waters Symmetry column. The mobile phase consisted of 0.02 M sodium dodecyl sulfate + 0.3% triethylamine + 10% n-propanol, prepared in 0.02 M orthophosphoric acid. The pH of the mobile phase was adjusted to pH 6.0, and it was pumped at a flow rate of 0.7 mL/min with UV detection at 262 nm. The method showed good linearity in the range of 2-80 microg/mL, with an LOD of 0.40 microg/mL (1.31 x 10(-6) M) and an LOQ of 1.21 microg/mL. The suggested method was successfully applied for the analysis of risedronate in raw material and a tablet formulation, with average recoveries of 99.91 +/- 1.30 and 101.52 +/- 0.30%, respectively. The stability-indicating capability of the proposed method was proved using forced degradation. By changing the pH of the mobile phase to 4.0, the oxidative degradation product could be separated from risedronate.     

Factors affecting optical dispersion in borate glass systems

Series of ternary glass systems namely, Na₂O, B₂O₃, and RO (R=Ba or Mg) doped with TiO₂ are synthesized. The present glasses are dictated by requirement for a small refractive index and a small nonlinear coefficient needed for waveguide and laser fabrication requirements. The effect of MgO and BaO as alkaline earth metals on the optical properties of the glass systems is investigated. The dependence of the refractive index and extinction coefficient dispersion curves on composition is carried out over a wavelength range of 0.3-. Applying a genetic algorithm technique, the parameters of Sellmeier dispersion formula that fit index data to accuracy consistent well with the measurements are given. The zero material dispersion-wavelength (ZMDW) and group velocity are also determined using the refractive index data. The Fermi level is calculated exploiting the extinction coefficient dispersion curves. The absorption coefficient, both direct and indirect optical energy gaps, and Urbach energy are evaluated using the absorption edge calculations. The different factors that play a role for controlling the refractive indices such as coordination number, electronic polarizability, field strength of cations, bridging and nonbridging oxygen, and optical basicity are discussed in accordance with the obtained index data. IR spectroscopy is used as a structural probe of the nearest-neighbor environment in the glass network.     

Synthesis of polyamidoamine dendrimer (PAMAM/CuS/AA) nanocomposite and its application in the removal of Isma acid fast yellow G Dye

The adsorption of Isma acid fast yellow G dye was studied using polyamidoamine (PAMAM)/Copper sulfide (CuS)/AA nanocomposite containing different amounts of CuS by batch technique. PAMAM dendrimer/CuS/AA nanocomposites were synthesized via gamma irradiation cross‐linking method with the aid of sonication. The nanocomposites were characterized by Fourier‐transform infrared, X‐ray diffraction, transmission electron microscope, energy dispersive spectroscopy X‐ray, thermal gravimetric analysis, ultraviolet‐visible, and fluorescence spectroscopy. The size of the CuS nanoparticles was formed in the range of 12–19 nm. The adsorption capacity of the nanocomposites was evaluated as a function of initial dye concentration, pH, adsorbent dosage, and time. It was verified that the adsorption rate fits a pseudo‐second‐order kinetics for initial Isma acid fast yellow G dye concentrations. Results indicated that the adsorption of Isma acid fast yellow G dye fitted well to the Langmuir model. Our results demonstrate that the PAMAM dendrimer/CuS/AA nanocomposite is very promising for removing organic dyes from wastewater. Copyright © 2015 John Wiley & Sons, Ltd.     

Simultaneous HPLC determination of thiocolchicoside and glafenine as well as thiocolchicoside and floctafenine in their combined dosage forms

Sensitive and accurate high-performance liquid chromatographic methods have been developed for the simultaneous determination of thiocolchicoside (TC)-glafenine (GF) (Mix I) and thiocolchicoside-floctafenine (FN) (Mix II) in their pharmaceutical formulations. The analysis for both mixtures was performed using 250 mm × 4.6 mm i.d., 5 μm particle size C18 Waters Symmetry column. The mobile phase consisted of methanol-0.035 M phosphate buffer (50:50, v/v) of pH 4.5 for Mix I and methanol-0.03 M phosphate buffer (70:30, v/v) of pH 4 for Mix II with flow rate of 1 mL/min and UV detection at 400 nm in both cases. The calibration plots were rectilinear over the concentration range of 0.2-2 μg/mL for TC in both mixtures and 20-200 μg/mL for each of GF and FN . The limits of detection for TC and GF were 0.05 μg/mL and 0.62 μg/mL, respectively, and for TC and FN were 0.02 μg/mL and 0.70 μg/mL, respectively. Additionally, the proposed methods were successfully applied to their combined tablets with average percentage recoveries of 100.35 ± 0.61 and 100.57 ± 0.72% for TC and GF respectively and for TC and FN the percentage recoveries were 101.2 ± 0.72 and 100.36 ± 0.67%, respectively. The results obtained were favorably compared with those given using the comparison methods.     

On/off luminescence vapochromic selective sensing of benzene and its methylated derivatives by a trinuclear silver(I) pyrazolate sensor

{[3,5-(CF(3))(2)Pz]Ag}(3) (1) films exhibit selective/reversible sensing of small-organic-molecule (SAM) vapors, which readily switch-on bright-green (benzene or toluene) or bright-blue (mesitylene) luminescence that switches-off upon vapor removal. Vapors of electron-deficient SAMs or non-aromatic solvents did not attain luminescence switching and were not adsorbed.     

Activity of Compounds from Temperate Propolis against Trypanosoma brucei and Leishmania mexicana

Ethanolic extracts of samples of temperate zone propolis, four from the UK and one from Poland, were tested against three Trypanosoma brucei strains and displayed EC₅₀ values < 20 µg/mL. The extracts were fractionated, from which 12 compounds and one two-component mixture were isolated, and characterized by NMR and high-resolution mass spectrometry, as 3-acetoxypinobanksin, tectochrysin, kaempferol, pinocembrin, 4′-methoxykaempferol, galangin, chrysin, apigenin, pinostrobin, cinnamic acid, coumaric acid, cinnamyl ester/coumaric acid benzyl ester (mixture), 4′,7-dimethoxykaempferol, and naringenin 4′,7-dimethyl ether. The isolated compounds were tested against drug-sensitive and drug-resistant strains of T. brucei and Leishmania mexicana, with the highest activities ≤ 15 µM. The most active compounds against T. brucei were naringenin 4′,7 dimethyl ether and 4′methoxy kaempferol with activity of 15–20 µM against the three T. brucei strains. The most active compounds against L. mexicana were 4′,7-dimethoxykaempferol and the coumaric acid ester mixture, with EC₅₀ values of 12.9 ± 3.7 µM and 13.1 ± 1.0 µM. No loss of activity was found with the diamidine- and arsenical-resistant or phenanthridine-resistant T. brucei strains, or the miltefosine-resistant L. mexicana strain; no clear structure activity relationship was observed for the isolated compounds. Temperate propolis yields multiple compounds with anti-kinetoplastid activity.     

Glycerol: A Promising Benign Solvent for Catalyst‐free One‐pot Multi‐component Synthesis of 1H‐Pyrozolo[1,2‐b]phthalazine‐5,10‐diones and 2H‐Indazolo[2,1‐b]phthalazine‐triones Under Controlled Microwaves Irradiation

A simple green and efficient one‐pot multi‐component synthesis of 1H‐pyrozolo[1,2‐b]phthalazine‐5,10‐diones and 2H‐indazolo[2,1‐b]phthalazine‐triones has been developed utilizing one‐pot multi‐component reaction of aromatic aldehydes, active methylene reagents, phthalic anhydride, and hydrazine hydrate or alternatively phthalhydrazide in glycerol without catalyst under controlled microwave heating. The current synthetic protocol offers several advantages such as excellent yields, high EcoScale and atom economy, simple working up reactants and products, and the absence of hazardous catalysts or solvents.     

Effect of γ-irradiation on slow crack growth in a copolymer of polyethylene

The effect of γ-irradiation on slow crack growth (SCG) in a medium density polyethylene (MDPE) was measured and compared with behavior of high density polyethylene (HDPE) and a recrystallized HDPE (RCHDPE). The three materials exhibited the same dependence on dose up to 3 Mrd. The HDPE became brittle above 50 Mrd. The resistance to SCG of MDPE and RCHDPE increased very rapidly with dose above 3 Mrd, until at 50–80 Mrd their resistance to SCG became extraordinarily high. This high resistance to SCG was accompanied by a transition from crazing to shear deformation at the root of a notch. It was found that for the same concentration, crosslinks are more effective than short chain branches for increasing resistance to SCG. © 1998 John Wiley & Sons, Inc. J. Polym. Sci. B Polym. Phys. 36: 2349–2354, 1998