A validated stability-indicating RP-HPLC assay method for Amsacrine and its related substances

A validated specific stability indicating reversed-phase high-performance liquid chromatography method was developed for the quantitative determination of Amsacrine as well as its related substances determination in bulk samples, in presence of degradation products, and its process related impurities. Forced degradation studies were performed on bulk samples of Amsacrine as per International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human use (ICH) prescribed stress conditions using acid, base, oxidative, thermal stress, and photolytic degradation to show the stability indicating power of the method. Significant degradation was observed during basic hydrolysis, slight degradation was observed in oxidative and thermal stress, and no degradation was observed in other stress conditions. The chromatographic method was optimized using the samples generated from forced degradation studies and the impurity spiked solution. Good resolution between the peaks corresponds to process-related impurities and degradation products from the analyte were achieved on Inertsil ODS column using the mobile phase consists a mixture of 1.0% triethyl amine in 20 mM potassium dihydrogen orthophosphate, with pH adjusted to 6.5, with ortho phosphoric acid in water and acetonitrile using a simple linear gradient. The detection was carried out at wavelength 248 nm. The mass balance in each case was in between 99.4% to 99.9%, indicating that the developed method was stability-indicating. Validation of the developed method was carried out as per ICH requirements. The developed method was found to be suitable to check the quality of bulk samples of Amsacrine at the time of batch release and also during its stability studies.     

Levitin–Polyak well-posedness for parametric quasivariational inequality problem of the Minty type

In this paper, we introduce the notions of Levitin?CPolyak (LP) well-posedness and Levitin?CPolyak well-posedness in the generalized sense, for a parametric quasivariational inequality problem of the Minty type. Metric characterizations of LP well-posedness and generalized LP well-posedness, in terms of the approximate solution sets are presented. A parametric gap function for the quasivariational inequality problem is introduced and an equivalence relation between LP well-posedness of the parametric quasivariational inequality problem and that of the related optimization problem is obtained.     

A Validated, Specific Stability-Indicating RP-LC Method for Moxifloxacin and Its Related Substances

A validated, specific, stability-indicating reversed-phase liquid chromatographic method has been developed for quantitative analysis of moxifloxacin and its related substances in bulk samples and pharmaceutical dosage forms in the presence of degradation products and process-related impurities. Forced degradation studies were performed on bulk samples of moxifloxacin, in accordance with ICH guidelines, using acidic, basic, and oxidizing conditions, and thermal and photolytic stress, to show the stability-indicating power of the method. Significant degradation was caused by oxidative stress and by basic conditions; no degradation was observed under the other stress conditions. The method was optimized by analysis of the samples generated during the forced degradation studies and sample solutions spiked with the impurities. Good resolution between the analyte peak and peaks corresponding to process-related impurities and degradation products was achieved on a C₁₈ column with a simple linear mobile phase gradient prepared from aqueous sodium dihydrogen orthophosphate dihydrate containing triethylamine, pH adjusted to 3.0 with orthophosphoric acid, and methanol. Detection was performed at 240 nm. Limits of detection and quantification were established for moxifloxacin and its process related impurities. When the stressed test solutions were assayed against moxifloxacin working standard solution the mass balance was always between 99.3 and 100.1%, indicating the method was stability-indicating. The method was validated in accordance with ICH guidelines, and found to be suitable for checking the quality of bulk samples of moxifloxacin at the time of release of a batch and during storage (long term and accelerated stability testing was conducted).     

Recent advances in heterogeneous catalysts for the synthesis of imidazole derivatives

Among the bioactive heterocyclic frameworks, nitrogen containing multisubstituted imidazoles are versatile building blocks of many naturally occurring products. Imidazoles possess wide range of biological properties including anticancer, anti-inflammatory, antimicrobial, and antihypertensive activities with potential applications in other sectors. Multicomponent reactions in combination with heterogeneous catalysts and nanocomposites have contributed significantly to organic synthesis in general and imidazoles, in particular with high functional group tolerance. Owing to their tunable properties, lower operational cost, thermal stability, recyclability, and easily separation from products, heterogeneous catalysts and nanocomposites are integral part of numerous pharmaceutical, agrochemical, and industrial processes. There has been increased focus on the development of green and sustainable catalytic procedures for the building of novel and biologically potent imidazole conjugates. This article emphasizes the recent advances in recyclable catalysts and protocols, and their merits for the synthesis of diverse multisubstituted imidazole conjugates by one-pot reaction approach and the catalyst and reactant interactions.     

Radiation-Induced Copolymerization of Acrylonitrile with Methyl Acrylate: Synthesis and Characterization

Radiation-induced copolymerization of acrylonitrile with methyl acrylate was carried out in aqueous medium at room temperature. Different compositions of the copolymer were prepared and characterized by IR, ¹H-NMR, thermal, and dielectric studies. NMR spectroscopy was used to determine the composition and stereochemistry of the copolymer. Glass transition temperature values (T_g ) were determined by DSC. Dielectric studies were carried out to understand the segmental motions and the effect of composition on dielectric loss.     

Structure-reactivity correlation in bromate oscillatory systems in aqueous-acetonitrile mixed medium

The oscillatory behavior of eight substrates has been studied in the uncatalyzed and catalyzed [Mn(II) and ferroin] bromate systems in aqueous-acetonitrile mixed medium. The reactivities of structurally related compounds are correlated using their oscillatory characteristics. The exchange current density values of the redox couples involved play a vital role in deciding the oscillatory characteristics of the system.     

Iodine-catalyzed one-pot synthesis of amides from nitriles via Ritter reaction

Ritter reactions of alcohols and tert-butyl acetate with various nitriles were performed using iodine as a mild and effective catalyst under heating conditions to afford the corresponding amides in good to excellent yields.     

Zeolite H‐Y–Supported Copper(II) Nitrate: A Simple and Effective Solid‐Supported Reagent for Nitration of Phenols and Their Derivatives

Highly regiospecific mononitration of phenols and substituted phenols is accomplished by employing copper(II) nitrate supported on a catalytic amount of zeolite H‐Y in a solid state.     

Vanadyl(IV) Acetate: An Efficient,Reusable Heterogenous Catalyst for Aza-Michael Reaction Under Solvent-Free Conditions

Vanadyl(IV) acetate [VO(OAc)₂] efficiently catalyzes the conjugate addition of aliphatic, aromatic amines to α,β-unsaturated carbonyl compounds in solvent-free media at room temperature to afford corresponding amino compounds in good to excellent yields. The catalyst can be recovered and reused for further cycles.