A FAST AND SENSITIVE SPECTROPHOTOMETRIC METHOD FOR THE DETERMINATION OF HYDRAZINE IN ATAZANAVIR SULFATE DRUG SUBSTANCE

Objective: To develop a fast and sensitive UV spectrophotometric method for the quantitative estimation of Hydrazine in Atazanavir Sulfate drug substances and validate as per ICH guidelines. Methods: The method was based upon the observation, that a characteristic colour results upon addition of a solution of p-Dimethylaminobenzaldehyde in ethyl alcohol and hydrochloric acid to hydrazine and estimated at absorbance maximum  458 nm in Atazanavir drug substance. Results: The developed method resulted in Hydrazine exhibiting linearity in the range 0.2 to 2.7 µg/g. The Intraday and interday precision is exemplified by relative standard deviation of 0.959 % and 0.947%. Percentage Mean recovery was found to be in the range of 97â€101%, during accuracy studies. The limit of detection (LOD) and limit of quantitiation (LOQ) were found to be 0.2 µg/g and 0.6 µg/g respectively. Conclusion: The present work was aimed to develop a visible spectrophotometric method, which is simple, sensitive, accurate and cost effective to evaluate the quality of the bulk and pharmaceutical formulations

Validated Method for the Determination of Five Membered Heterocyclic Polar Compound Imidazole in Drug Substances Using Capillary Electrophoresis and UV Detection

A simple and sensitive method based on capillary electrophoresis with UV detection was developed, optimized, and validated for the determination of five membered heterocyclic polar compound, imidazole in pharmaceutical drug substances. Separation was achieved on bare fused silica capillary using a simple running buffer, potassium dihydrogen phosphate at pH 4.0. Capillary temperature set at 25°C. The applied voltage was 25 kV across the capillary and the samples were injected by hydrodynamically at a pressure of 50 mbar for 5 s. Analyte was monitored at 210 nm. The achieved limit of detection value was 0.005%w/w, limit of quantification value was 0.014%w/w, and the average accuracy value was 98.4% for imidazole. The aim of present study is to develop a specific and sensitive method for the determination of imidazole to overcome the void volume and sample matrix interferences

Synthesis of compounds related to the anti-migraine drug eletriptan hydrobromide

Eletriptan hydrobromide (1) is a selective serotonin (5-HT1) agonist, used for the acute treatment of the headache phase of migraine attacks. During the manufacture of eletriptan hydrobromide the formation of various impurities were observed and identified by LC–MS. To control the formation of these impurities during the preparation of active pharmaceutical ingredients, the structure of the impurities must be known. Major impurities of the eletriptan hydrobromide synthesis were prepared and characterized by using various spectroscopic techniques, i.e., mass spectroscopy, FTIR , 1H NMR, 13C NMR/DEPT, and further confirmed by co-injection in HPLC. The present study will be of great help in the synthesis of highly pure eletriptan hydrobromide related compounds

Resolution of racemic Vigabatrin using tartaric acid

<p>An efficient and simple resolution methodology for the preparation of (<i>S</i>)- and (<i>R</i>)-Vigabatrin has been developed. In addition, a method of preparation for the novel compounds Vigabatrin-l-tartarate and Vigabatrin-d-tartarate is also described. The title compounds have been synthesized via resolution of Vigabatrin using commercially available l-(+)- and d-(−)-tartaric acids respectively.</p

Design and applications of new phosphine-free tetradentate Pd-catalyst: Regioselective C–H activation on 1-substituted 1,2,3-triazoles and indoles(NH-Free)

<p>This article describes the synthesis of a new phosphine free tetradentate Pd catalyst using dl-2,3-diaminopropionic acid. The complex was characterized by Mass, IR, and ¹H NMR. The catalyst is air stable at room temperature and non-hygroscopic. Application of this new catalyst to regioselective C–H activation on 1-substituted 1,2,3-triazole and indoles with aryl iodides to get corresponding C-5 and C-2 arylated products with satisfactory yields. All the products were characterized by spectroscopic studies.</p

An Improved Process for the Preparation of Highly Pure Solifenacin Succinate via Resolution through Diastereomeric Crystallisation

An improved process for the preparation of solifenacin succinate (<b>1</b>) involving resolution through diastereomeric crystallization is described. (1<i>S</i>)-IQL derivative (<b>5</b>) is esterified to form (1<i>S</i>)-ethoxycarbonyl IQL derivative (<b>6</b>) which is condensed with (<i>RS</i>)-3-quinuclidinol (<b>7</b>) to form a solifenacin diastereomeric mixture (<b>8</b>); this is subjected to resolution through diastereomeric crystallization to produce solifenacin succinate (<b>1</b>), which is used for the treatment of an overactive bladder