Spectrophotometric Methods for the Determination of Chloramphenicol,Dexamethasone Sodium Phosphate,and Tetrahydrozoline HCl in their Pure and Ophthalmic Dosage Forms

Journal of Applied Spectroscopy - Chloramphenicol (CHL), dexamethasone sodium phosphate (DSP), and tetrahydrozoline HCl (THZ) are co-formulated for conjunctivitis treatment. The ternary mixture...     

Stability assessment of FDA-approved ramucirumab monoclonal antibody; validated SE-HPLC method for degradation pattern evaluation

Ramucirumab (RAMU) is a recently US Food and Drug Administration-approved monoclonal antibody that is included in various anticancer protocols. It has a structural complexity and high degradation risk that have a significant effect on its safety and effectiveness. The major aim of this work was to assess the degradation pattern of RAMU based on physicochemical characterization. Mechanical agitation, repeated freeze–thaw cycles, pH and temperature were the selected stress conditions to which RAMU samples were subjected. The SE-HPLC method was applied and validated to monitor the RAMU monomer along with its aggregates and/or fragments. The purity of the separated peaks together with system suitability parameters were determined through the calculation of percentage purity and percentage drop in RAMU concentration. The results were interpreted by correlating them with those of dynamic light scattering and reducing and non-reducing sodium dodecyl sulfate–polyacrylamide gel electrophoresis. Samples incubated at pH 2.0–10.0 and 37°C for up to 4 weeks were analysed, recording detection of reversed phase (RP) aggregates and low molecular weight peptide fragments. Similarly, samples under short-term storage conditions of 4 weeks at different temperatures (−20, 2–8, 25, 37 and 50°C) showed low molecular weight peptide fragments but to a lesser extent. These results highlight the alarming effect on RAMU multidose vial efficacy and safety.     

Voltammetric Determination of Oxybutynin Hydrochloride Utilizing Pencil Graphite Electrode Decorated with Gold Nanoparticles

A novel voltammetric method was successfully applied for the determination of an anticholinergic drug, oxybutynin hydrochloride (OXB). The method is concerned with electrooxidation of the drug on the surface of pencil graphite electrode (PGE). In order to enhance the electrode sensitivity and peak current, the electrode was coated with gold nanoparticles (Au-NPs) via electrochemical deposition using cyclic voltammetry from gold salt solution. The surface of Au-NPs modified PGE has been characterized using scanning electron microscopy and X-ray photoelectron spectroscopy. Various experimental variables were studied and optimized to enhance the sensor's response towards OXB. Quantitative determination of the drug was achieved in phosphate buffer pH 7.5 using differential pulse voltammetry by scanning the potential over range of 0.00 to 2.20 V with scan rate of 40 mV s⁻¹. Validation of the method was achieved according to ICH guidelines. The method was found to be linear over concentration range (2.0×10⁻⁷–1.0×10⁻⁶ M). The suggested sensor was efficiently developed for the quantitative determination of OXB in pure form, pharmaceutical dosage form and spiked plasma samples.     

A comparative study of surface acidity in the amorphous, high surface area solids, aluminium fluoride, magnesium fluoride and magnesium fluoride containing iron(III) or aluminium(III) fluorides

The behaviour of the sol–gel prepared, amorphous solids, high surface area (HS) aluminium fluoride and magnesium fluoride in promoting room temperature dehydrochlorination of tert-butyl chloride (Bu^tCl), in their catalytic activity for the dismutation of chlorodifluoromethane and in the temperature programmed desorption of ammonia is similar, indicating that, unexpectedly, both solids exhibit significant surface Lewis acidity. Using a similar approach, it has been demonstrated that surface Lewis acidity in HS-MgF₂ is enhanced by the incorporation of amorphous iron(III) fluoride and probably also by amorphous aluminium(III) fluoride. A second, unexpected feature is the substantial retention of anhydrous hydrogen chloride by all the solids, which is observed by the use of chlorine-36 labelling, when they are exposed at room temperature either to Bu^tCl or to HCl directly. The detailed behaviour of H³⁶Cl towards HS-AlF₃ depends on the fluorinating agent, dichlorodifluoromethane or anhydrous hydrogen fluoride, which is used in the second stage of HS-AlF₃ synthesis. This observation and the pattern of the results obtained overall lead to the proposal that strongly adsorbed HCl behaves as an unconventional Lewis base towards these solids.     

Real sol-gel synthesis of catalytically active aluminium fluoride

Abstract Amorphous AlF₃ prepared via an anhydrous sol-gel synthesis route exhibits high surface area and Lewis acidity far beyond those known for crystalline AlF₃ phases. Its catalytic properties are comparable to those of SbF₅. Basis of its unusual properties is a sol-gel fluorination with anhydrous HF in organic solvents yielding first a wet Al-F-sol-gel, which can be dried and eventually post-fluorinated. All parts of the synthesis route were thoroughly investigated. The results of these investigations together with detailed analysis of the Al-F-materials obtained are reported and discussed.