Stability-indicating high-performance thin-layer chromatography method for the simultaneous estimation of emtricitabine and tenofovir alafenamide fumarate

A simple, precise, rapid and accurate high-performance thin-layer chromatographic method was developed and validated for the simultaneous estimation of emtricitabine (EMT) and tenofovir alafenamide fumarate (TAF) in combined dosage forms and forced degradation studies were carried out as per the International Council for Harmonisation (ICH) guidelines. The stationary phase used was Merck TLC silica gel 60 F₂₅₄ aluminum plates. The mobile phase used was ethyl acetate‒n-hexane‒methanol‒ammonia solution (4:4:2:0.2, V/V). Densitometric evaluation was carried out at 260 nm, EMT and TAF. The concentration ranges used for the study are 400–2000 ng/band for EMT, 50–250 ng/band for TAF. EMT and TAF gave well defined and sharp peaks at retardation factor 0.43 and 0.56, respectively. The stability study showed that samples degraded with acid, base, hydrogen peroxide and light gave well separated peaks of EMT and TAF as well as some additional peaks at different retardation factor values. The proposed method is simple, suitable, accurate and stable in accordance with the ICH guidelines.

     

Evolution of texture and grain boundary microstructure in two-phase (α + β) brass during recrystallization

The evolution of texture and microstructure during recrystallization is studied for two-phase copper alloy (Cu–40Zn) with a variation of the initial texture and microstructure (hot rolled and solution treated) as well as the mode of rolling (deformation path: uni-directional rolling and cross rolling). The results of bulk texture have been supported by micro-texture and microstructure studies carried out using electron back scatter diffraction (EBSD). The initial microstructural condition as well as the mode of rolling has been found to alter the recrystallization texture and microstructure. The uni-directionally rolled samples showed a strong Goss and BR {236}?385? component while a weaker texture similar to that of rolling evolved for the cross-rolled samples in the α phase on recrystallization. The recrystallization texture of the β phase was similar to that of the rolling texture with discontinuous ?101? α and {111} γ fiber with high intensity at {111}?101?. For a given microstructure, the cross-rolled samples showed a higher fraction of coincident site lattice Σ3 twin boundaries in the α phase. The higher fraction of Σ3 boundaries is explained on the basis of the higher propensity of growth accidents during annealing of the cross-rolled samples. The present investigation demonstrates that change in strain path, as introduced during cross-rolling, could be a viable tool for grain boundary engineering of low SFE fcc materials.     

Working group report: High energy and collider physics

This is a summary of the projects undertaken by the working group I on high energy and collider physics.     

The Mixing Effect of Glycylglycine with KCl, KBr, and Na2SO4 from Volumetric and Viscometric Investigations at 298.15 K

The mixing effect of a simple peptide such as glycylglycine, in the presence of aqueous electrolytes, has been studied by examining their volumetric and viscometric behavior. The increase in the apparent molar properties of both glycylglycine and electrolytes is attributed to the interactions present among cation, anion, the head groups of the peptide, and the peptide bond. Simple equations are developed to account for such interactions with a view to correlate apparent molar properties of glycylglycine and electrolyte in their aqueous mixtures. Transfer properties of both glycylglycine and electrolyte are investigated in order to understand the changes in the property of one component by the addition of another. These interactions are also supported by viscosity data, for which a simple model is developed to correlate the variation in viscosities with composition of a component.     

Differential electrochemical behaviour of phytofabricated and chemically synthesized silver nanoparticles towards hydrogen peroxide sensing**

Silver nanoparticles (AgNPs) are one of the most widely used nanomaterials for biomedical applications. However, the impact of its synthesis by chemical and plant-mediated routes on its differential electrochemical behaviour has not been examined till date. Here, we report for the first time the differential study of the electrochemical behaviour of the AgNPs synthesized by different routes. First, the AgNPs were obtained by different routes (chemical and phytofabrication) and extensively characterized to compare their physical properties. Thereafter, a comparison of electron transfer kinetics between chemically synthesized (Ag−C) and phyto-fabricated (Ag-Phy) nanoparticles (NPs) has been studied by electrochemical techniques such as potentiodynamic cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). To further investigate the electrocatalytic properties of both types of AgNPs, we have used the peroxide moieties (H₂O₂), and the Ag−C NPs-based sensor probe has been reported to have four times better sensitivity than the Ag−Phy NPs-based sensor. The AgNPs modified sensor probes have also been tested in real-world environments to explore the consistency of their performance in complex matrices by using clinical urine samples, where we found comparable sensitivity to the standard conditions.     

Catalytic reduction of pralidoxime in pharmaceuticals by macrocyclic Ni(II) compounds derived from orthophthalaldehyde

Efficient catalytic method for the reduction of pralidoxime to its amine derivative by macrocyclic Ni(II) compounds has been developed. Ten macrocyclic Schiff base Ni(II) compounds were synthesized via non-template synthesis by treating the corresponding macrocycles with nickel chloride in 1:1 ratio. The resulting compounds were characterized by elemental, IR, (1)H NMR, (13)C NMR, mass, electronic spectra, conductance, magnetic, thermal studies and their structures have been proposed. These compounds were used as catalysts for the reduction of pralidoxime to its amino derivative. The reduced pralidoxime was also characterized by spectral analysis and catalytic cycle has been established. The reduced product was determined spectrophotometrically by treating with ninhydrin reagent and the percent yields were found to be in the range of 75.12-82.36%.