Stress Degradation Behavior of Entacapone and Development of LC Stability-Indicating Related Substances and Assay Method

A new, sensitive, stability indicating gradient RP-LC related substances and assay method has been developed for the quantitative determination of entacapone in bulk drugs. Efficient chromatographic separation was achieved on a C18 stationary phase with simple mobile phase combination of buffer and acetonitrile. Buffer consisted of 0.1% orthophosphoric acid, delivered in a gradient mode and quantitation was carried out using ultraviolet detection at 220 nm with a flow rate of 1.5 mL min^?1. In the developed LC method the resolution (R _s ) between entacapone and its three potential process impurities were found to be >2.0. Regression analysis showed an r ² value (correlation coefficient) >0.99 for entacapone and its three potential impurities. This method was capable to detect all three process impurities of entacapone at a level of 0.003% with respect to test concentration of 0.5 mg mL^?1 for a 20 μL injection volume. The inter- and intra-day precision values for all three impurities and for entacapone was found to be within 2.0% RSD. The method has shown good and consistent recoveries for entacapone in bulk drugs (99.2–101.5%) and its three impurities (99.5–102.2%). The test solution was found to be stable in diluent for 48 h. The drug substances were subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. Considerable degradation was found to occur in acid stress, base stress and oxidative conditions. The stressed test solutions were assayed against the qualified working standard of entacapone and the mass balance in each case was close to 99.7% indicating that the developed method was stability-indicating. The developed RP-LC method was validated with respect to linearity, accuracy, precision and robustness.     

Population balance models and Monte Carlo simulation for nanoparticle formation in water-in-oil microemulsions: implications for CdS synthesis

We address controlled CdS nanoparticle formation by tuning experimental synthesis conditions. To this end, a bivariate population balance equation (PBE) model has been developed based on time scale analysis, to explain the mechanism of nanoparticle formation in self-assembled templates. It addresses the process of mixing two water-in-oil (w/o) microemulsions, each containing a pre-dissolved reactant in the microemulsion drops. Brownian collision and coalescence of two water drops of nanometer size results in mixing and exchange of reactant molecules, leading to chemical reaction. The water insoluble reaction product nucleates to form a nanoparticle in an individual drop, which subsequently grows internally by consuming the excess product and by coalescence-exchange with other drops. Finite rates of nucleation and coalescence-exchange are accounted for in the PBE, while the rates of reaction and internal growth of nanoparticles are found to be instantaneous. Experimentally proven binomial redistribution of reactant and product molecules upon drop coalescence is implemented in the present work. This results in a very good prediction of experimental data of the mean aggregate number (MAN) and hence size of CdS nanoparticles. Both our model and Monte Carlo (MC) simulation quantitatively capture the reported variation of MAN with molar excess of Cd2+ concentration and microemulsion drop size. Our results together with previous experimental data establish that usage of stoichiometrically five times or more of excess Cd2+ concentration can cause surface adsorption and desirable enhanced emission intensity of CdS nanoparticles, without altering particle size. We also propose a simplified and computationally efficient univariate PBE model. The univariate model gives very fast (in minutes) and accurate estimates (for low reactant concentrations) of the number and mean size of CdS nanoparticles. Time-scale analysis offers a good a priori choice of the appropriate model based on range of reactant concentrations.     

Computation of cascade flutter by uncoupled and coupled methods

A computational method for flutter prediction of turbomachinery cascades is presented. The flow through multiple blade passages is calculated using a time-domain approach with coupled aerodynamic and structural models. The unsteady Euler/Navier-Stokes equations are solved in quasi-three-dimensions using a second-order implicit scheme with dual time-stepping and a multigrid method. A structural model for the blades with bending and torsion degrees of freedom is integrated in time together with the flow field. Information between structural and aerodynamic models is exchanged until convergence in each real-time step. Computational results for a cascade are presented and compared with those obtained by the conventional energy method and with experimental and numerical data by other authors. Significant differences are found between the coupled and uncoupled methods at low mass ratios. A transonic test case with strong nonlinear phenomena is investigated with the fluid-structure coupled method. Results for inviscid flow are compared with results of Navier-Stokes computations.     

Nonlinear tunneling of optical soliton in 3 coupled NLS equation with symbolic computation

We investigated the soliton solution for N$N$ coupled nonlinear Schrödinger (CNLS) equations. These equations are coupled due to the cross-phase-modulation (CPM). Lax pair of this system is obtained via the Ablowitz–Kaup–Newell–Segur (AKNS) scheme and the corresponding Darboux transformation is constructed to derive the soliton solution. One and two soliton solutions are generated. Using two soliton solutions of 3 CNLS equation, nonlinear tunneling of soliton for both with and without exponential background has been discussed. Finally cascade compression of optical soliton through multi-nonlinear barrier has been discussed. The obtained results may have promising applications in all-optical devices based on optical solitons, study of soliton propagation in birefringence fiber systems and optical soliton with distributed dispersion and nonlinearity management.     

Nucleation kinetics,growth and hardness parameters of l-alanine alaninium picrate (LAAP) single crystals

Amino acids are considered to be the building blocks of proteins and are gaining importance due to their interesting optical behavior. l-alanine is an amino acid which dissolves in water and it can react with other acids to form new compounds. In this work, l-alanine is mixed with picric acid to prepare l-alanine alaninium picrate (LAAP) salt. Solubility and metastable zone width were measured for LAAP salt and induction period was measured at different supersaturation ratios. The critical nucleation parameters were evaluated based on the classical theory of homogeneous nucleation. Using the optimized nucleation parameters, single crystals of LAAP salt were grown by slow evaporation technique. XRD and FTIR studies were carried out to understand structural and molecular formation of the crystal. Microhardness measurements were performed on the grown LAAP crystal and various parameters such as work hardening constant, stiffness constant, yield strength, resistance pressure and corrected hardness were evaluated. Nonlinear optical behavior of the sample was analyzed.     

Stable-isotope dilution GC-MS method for ethanol in vapour ethanol and microdialysis systems based on carbonate-catalyzed extractive pentafluorobenzoylation

Common ethanol detection methods are not applicable to cell culture media and microdialysates due to interference with medium constituents including amino acids and pH indicators. We present a novel GC-MS method for the accurate and precise analysis of ethanol in cell cultures and microdialysates. The method is based on the carbonate-catalyzed extractive pentafluorobenzoylation of ethanol and deuterium-labelled ethanol serving as the internal standard and on their GC-MS analysis in the electron-capture negative-ion chemical ionization mode. The method was used to optimize experimental conditions in a custom-made ethanol vapour system utilized for studies examining ethanol influences on neuronal cell lines and in microdialysis.     

A study on the influence of dysprosium cation substitution on the structural, morphological, and electrochemical properties of lithium manganese oxide

The synthesis of series of dysprosium-doped lithium manganese oxide in the general formula LiDy _x Mn_2?x O4 (x?=?0.0, 0.05, 0.1, 0.15, and 0.2) using double stage coprecipitation method followed by microwave heat treatment is reported. The characterization results of X-ray diffraction and infrared spectroscopy have illustrated the cubic structure for all the compounds. The lattice parameter has been observed to decrease with dysprosium doping. The influence of doping in elastic property of the samples has been studied with infrared spectroscopy. The grain size of the LiDy_0.05Mn_1.95O₄ has been observed to be less than 1???m. The Image J software has been used to further analyze the micrographs. The initial capacity of the samples are observed to decrease with Dy³⁺ doping, but the capacity retention after 50 cycles for Dy 0.05, 0.1, 0.15, and 0.2 samples are reported as 95.4%, 93.2%, 91.3%, and 87.7%, respectively. The electrochemical impedance spectra has been performed to analyze the effectiveness of Dy³⁺ ion doping and the act of Dy doping has been observed to reduce the charge transfer resistance and increase the Li ion diffusion coefficient.     

Tunable energy transfer distributed feedback dye laser using pyronin B and crystal violet dye mixture

Using pyronin B and crystal violet dye mixture, the characteristics of energy transfer distributed feedback dye laser (ETDFDL) pumped by 532 nm Nd:YAG laser were investigated. The characteristics of donor DFDL and acceptor DFDL as well as the dependence of their pulse widths and output powers on pump power and acceptor concentrations were studied. The output energy of DFDL was measured at the emission peaks of donor and acceptor dyes for different pump powers and acceptor concentrations, and tunability was observed from 570 to 645 nm using prism dye cell arrangement.