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.     

Volumetric and transport properties of binary liquid mixtures of N-methylacetamide with lactones at temperatures (303.15 to 318.15) K

The values of density (ρ), viscosity (η) and speed of sound (u) have been measured for binary liquid mixtures of γ-butyrolactone (GBL), δ-valerolactone (DVL), and ε-caprolactone (ECL) with N-methylacetamide (NMA) over the whole composition range at T = (303.15 to 318.15) K and atmospheric pressure. From these data, excess molar volume (V^E), deviation in viscosity (Δη), and deviation in isentropic compressibility (Δκ_s), are calculated. The results are fitted to a Redlich–Kister type polynomial equation to derive binary coefficients and standard deviations.     

Benzoazabicyclo[4.3.1] derivatives by intramolecular Michael addition of piperidinone enolates to enoates

Piperidinones with a 2-bromobenzyl substituent in the 5-position were subjected to a Heck coupling reaction with ethyl acrylate resulting in the highly functionalized cinnamates 9a-d. A subsequent deprotonation of the piperidinones using NaN(SiM₃)₂ in THF induced an intramolecular Michael addition of the enolate to the cinnamate part. In this way, a range of novel 2,6-methano-4H-4-benzazonines 10-13 were obtained. In each case, a separable mixture of endo/exo-diastereomers was obtained.     

Lower bounds for adaptive locally decodable codes

An error‐correcting code is said to be locally decodable if a randomized algorithm can recover any single bit of a message by reading only a small number of symbols of a possibly corrupted encoding of the message. Katz and Trevisan 12 showed that any such code C : {0, 1}ⁿ → Σ^m with a decoding algorithm that makes at most q probes must satisfy m = Ω((n/log |Σ|)^q/(q?1)). They assumed that the decoding algorithm is non‐adaptive, and left open the question of proving similar bounds for adaptive decoders. We show m = Ω((n/log |Σ|)^q/(q?1)) without assuming that the decoder is nonadaptive. © 2005 Wiley Periodicals, Inc. Random Struct. Alg., 2005     

Efficient Approach to 4‐Benzyl‐5,5‐dimethyldihydrofuranones: Total Synthesis of (±_bold;)‐Solafuranone

A six‐step general and very efficient synthesis of 4‐(arylmethyl)‐5,5‐dialkyldihydrofuranones starting from corresponding aryl aldehyde has been developed. Solafuranone, a novel furanone isolated from the Chinese folk medicine Solanum indicum, has been accomplished starting from 2,6‐dimethylbenzaldehyde in six steps in an overall yield of 70%. Contrary to expectations, solafuranone and its analogue failed to exhibit any significant cytotoxicity against A549 (lung adenocarcinoma) and HL60 (leukemia cells) cell lines.     

Understanding guest and pressure‐induced porosity through structural transition in flexible interpenetrated MOF by Raman spectroscopy

Interpenetrating metal organic frameworks are interesting functional materials exhibiting exceptional framework properties. Uptake or exclusion of guest molecules can induce sliding in the framework making it porous or non‐porous. To understand this dynamic nature and how framework interaction changes during sliding, metal organic framework (MOF) 508 {Zn(BDC)( 4,4′‐Bipy)_0.5 · DMF(H₂O)_0.5} was selected for study. We have investigated structural transformation in MOF‐508 under variable conditions of temperature, pressure and gas loading using Raman spectroscopy and substantiated it with IR studies and density functional theory (DFT) calculations. Conformational changes in the organic linkers leading to the sliding of the framework result in changes in Raman spectra. These changes in the organic linkers are measured as a function of high pressure and low temperature, suggesting that the dynamism in MOF‐508 framework is driven by ligand conformation change and inter‐linker interactions. The presence of Raman signatures of adsorbed CO₂ and its librational mode at 149 cm⁻¹ suggests cooperative adsorption of CO₂ in the MOF‐508 framework, which is also confirmed from DFT calculations that give a binding energy of 34 kJ/mol. Copyright © 2015 John Wiley & Sons, Ltd.     

Large Time Asymptotics with Error Estimates to Solutions of a Forced Burgers Equation

This article deals with a forced Burgers equation (FBE) subject to the initial function, which is continuous and summable on . Large time asymptotic behavior of solutions to the FBE is determined with precise error estimates. To achieve this, we construct solutions for the FBE with a different initial class of functions using the method of separation of variables and Cole–Hopf like transformation. These solutions are constructed in terms of Hermite polynomials with the help of similarity variables. The constructed solutions would help us to pick up an asymptotic approximation and to show that the magnitude of the difference function of the true and approximate solutions decays algebraically to 0 for large time.     

An Improved Protocol for DNA Extraction from Alkaline Soil and Sediment Samples for Constructing Metagenomic Libraries

An improved single-step protocol has been developed for extracting pure community humic substance-free DNA from alkaline soils and sediments. The method is based on direct cell lysis in the presence of powdered activated charcoal and polyvinylpolypyrrolidone followed by precipitation with polyethyleneglycol and isopropanol. The strategy allows simultaneous isolation and purification of DNA while minimizing the loss of DNA with respect to other available protocols for metagenomic DNA extraction. Moreover, the purity levels are significant, which are difficult to attain with any of the methods reported in the literature for DNA extraction from soils. The DNA thus extracted was free from humic substances and, therefore, could be processed for restriction digestion, PCR amplification as well as for the construction of metagenomic libraries.