A Stability-Indicating LC Method for Analysis of Balsalazide Disodium in the Bulk Drug and in Pharmaceutical Dosage Forms

A novel, sensitive, stability-indicating gradient RP-LC method has been developed for quantitative analysis of balsalazide disodium and its related impurities both in the bulk drug and in pharmaceutical dosage forms. Efficient chromatographic separation was achieved on a C₁₈ stationary phase with a simple mobile-phase gradient prepared from methanol and phosphate buffer (10 mm potassium dihydrogen orthophosphate monohydrate, adjusted to pH 2.5 by addition of orthophosphoric acid). The mobile-phase flow rate was 1.0 mL min^?1. Quantification was achieved by use of ultraviolet detection at 240 nm. Under these conditions resolution of balsalazide disodium from its three potential impurities was greater than 2.0. Regression analysis resulted in a correlation coefficient greater than 0.99 for balsalazide disodium and all three impurities. This method was capable of detecting the three impurities at 0.003% of the test concentration of 0.3 mg mL^?1, using an injection volume of 10 μL. Inter-day and intra-day precision for all three impurities and for balsalazide disodium was within 2.0% RSD. Recovery of balsalazide disodium from the bulk drug (99.2–101.5%) and from pharmaceutical dosage forms (99.8–101.3%), and recovery of the three impurities (99.1–102.1%) was consistently good. The test solution was found to be stable in 70:30 (v/v) methanol–water for 48 h. When the drug was subjected to hydrolytic, oxidative, photolytic, and thermal stress, acidic and alkaline hydrolysis and oxidizing conditions led to substantial degradation. The RP-LC method was validated for linearity, accuracy, precision, and robustness.     

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.     

Structure elucidation of an unexpected product from dehydration of a beta-hydroxyketone

The structure of an unexpected compound from the dehydration of an aldol addition product has been determined using 1-D and 2-D NMR techniques. This reaction is the last step in a new synthetic approach to the galanthan ring system. Complete 1H and 13C NMR assignments for two synthetic precursors are also reported.     

Numerical investigation of coexisting high and low amplitude responses and safe basin erosion for a coupled linear oscillator and nonlinear absorber system

Over the last half century, numerous nonlinear variants of the tuned mass damper have been developed in order to improve attenuation characteristics. In the present study, the performance of a linear oscillator and an absorber with a strongly nonlinear cubic stiffness is evaluated by using numerical methods. This configuration has been of recent interest due to its capability of wide-band energy absorption. However, high amplitude solutions, which would amplify the response of the system, have been shown to often coexist with the low amplitude solutions. The present research is focused on numerically determining the relative strength of the coexisting solutions. Erosion profiles are presented, quantifying the integrity of the system, i.e. the likelihood of converging to a safe, low amplitude response, and providing an indication of the structural safety of a practical absorber system. The results indicate that the high amplitude solutions not only exist but significantly influence the response of the system within the range of expected operating conditions, particularly at excitation frequencies lower than the natural frequency of the linear oscillator. The erosion profiles indicate a 20–40% increase in system integrity for the case of zero damping compared to a small amount of damping, no significant integrity change when adding a small linear stiffness component to the nonlinear absorber, and no significant change in integrity between the midpoint and extreme of the bi-stable range. Additional higher-period solutions are also discovered and evidence of a chaotic response is presented.     

Fluoranthene based fluorescent chemosensors for detection of explosive nitroaromatics

A novel fluoranthene based fluorescent chemosensor for the detection of picric acid (PA) at the parts per billion (ppb) level was evaluated. Static fluorescence quenching was the dominant process by intercalative π-π interaction between fluoranthene (S(1)) and nitroaromatics.     

Recoverable and thermally stable superhydrophobic silica coating

A facile route to methyltrimethoxysilane (MTMS) based recoverable superhydrophobic silica coatings with dual-scale roughness obtained through the single step base catalyst sol–gel process. Superhydrophobic silica coatings have shown static water contact angle near about 170 ± 1° and dynamic water contact angle up to 2 ± 1°. Superhydrophobic-superhydrophilic switching feature also achieved by alternating heat treatment and bath surface modification with Trimethylchlorosilane (TMCS) at room temperature (26 °C). Furthermore, the superhydrophobic state could be transformed into superhydrophilic state by slow rate heat treatment. These studies present a very simple strategy for the fabrication of recoverable superhydrophobic surfaces.     

Study of physical chemistry on biosorption of zinc by using Chlorella pyrenoidosa

Discharge of heavy metals from metal processing industries is known to have adverse effects on the environment. Biosorption of heavy metals by metabolically inactive biomass of microbial organisms is an innovative and alternative technology for removal of these pollutants from aqueous solution. Presence of heavy metals in the aquatic system is posing serious problems. Zinc has been used in many industries and removal of Zn ions from waste water is significant. Biosorption is one of the economic methods used for removal of heavy metals. In the present study, the biomass obtained from the dried Chlorella pyrenoidosa was used for evaluating the biosorption characteristics of Zn ions in aqueous solutions. Batch adsorption experiments were performed with this material and it was found that the amount of metal ions adsorbed increased with the increase in the initial metal ion concentration. In this study effect of agitation time, initial metal ion concentration, temperature, pH and biomass dosage were studied. Maximum metal uptake (q _max) observed at pH 5 was 101.11 mg/g. The biosorption followed both Langmuir and Freundlich isotherm model. The adsorption equilibrium was reached in about 1 h. The kinetic of biosorption followed the second-border rate. The biomass could be regenerated using 0.1 M HNO₃. A positive value of ΔH° indicated the endothermic nature of the process. A negative value of the free energy (ΔG°) indicated the spontaneous nature of the adsorption process. A positive value of ΔS° showed increased randomness at solid-liquid interface during the adsorption of heavy metals, it also suggests some structural changes in the adsorbate and the adsorbent. FTIR Spectrums of Chlorella pyrenoidosa revealed the presence of hydroxyl, amino, carboxylic and carbonyl groups. The scanning electron micrograph clearly revealed the surface texture and morphology of the biosorbent.     

Microwave assisted mild, rapid, solvent-less, and catalyst-free chemoselective N-tert-butyloxycarbonylation of amines

Microwave assisted simple, rapid, solventless, and catalyst-free chemoselective method for the protection of amino group in aromatic, aliphatic, heterocyclic, aralkyl amines, phenyl hydrazine, and amino acid esters in good to excellent isolated yield (83-98%) in short reaction time (2-12 min) has been reported.     

Thin-film models of liquid displacement on chemically patterned surfaces for lithographic printing processes

We examine in this work a model problem relevant to the liquid displacement that occurs in lithographic printing processes. The model problem consists of two stratified thin liquid films confined between parallel plates, one of which is chemically heterogeneous. The films are assumed to be thin enough so that intermolecular forces are important and the lubrication approximation can be invoked. Both linear stability analysis and nonlinear simulations are applied to a partial differential equation governing the behavior of the liquid-liquid interface. The results provide physical insights into and numerical estimates of the smallest and largest feature sizes that can be printed, as well as the minimum spacing between feature sizes that can be tolerated. The results also provide insight into experimental observations on a closely related process, wire-wound rod coating on chemically patterned surfaces. The work presented here has important implications for the production of electronic devices and displays by lithographic printing, as well as for other processes that rely on coating and printing on chemically patterned surfaces.