Stability indicating method.

To develop a new, economical, precise and accurate stability indicating HPTLC method was developed and validated for the determination of Adapalene in bulk drug. The present study deals with development and validation of stability indicating HPTLC method for estimation of Adapalene. Chromatographic separation was performed on aluminium plate pre-coated with Silica Gel 60 F254 using Tetrahydrofuran: 2-Propanol: Water (3:3:3 v/v/v) as a mobile phase. The wavelength selected for densitometric scanning was 230 nm. Regression plots revealed linear relationship in the concentration range of 20-120 ng spot-1. The Rf value of Adapalene was found to be 0.76 (±0.02).The LOD and LOQ were found to be 3.15 and 9.57 ng spot-1respectively. The method was validated as per International Conference on Harmonization (ICH) guidelines, demonstrating to be accurate and precise within the corresponding linearity range of titled analytes. Inherent stability of the drug was studied by exposing drug to acid, alkali, oxidative, photolytic and thermal conditions. Relevant degradation was found to take place under these conditions. The proposed method has been validated as per ICH Q2 (R1) guidelines. This method can be used for routine quality control analysis of Adapalene in bulk drug.

A Novel stability-indicating method was developed and validated by Reverse phase Hplc method   for the estimation of Thiotepa in Lyophilized form. The simple, Accurate Assay method was developed by PDA Detector at 215nm and column(YMC,150mmx4.6mm, 3.5 μm,12nm).The mobile phase A consisted of (3.5g of potassium Dihydrogen phosphate/1liter: 4.2g of Disodium hydrogen Phosphate/2liters)Buffer : Acetonitrile (85:15v/v) and The mobile phase B consisted of (3.5g of potassium Dihydrogen phosphate/1liter: 4.2g of Disodium hydrogen Phosphate/2liters)Buffer : Acetonitrile (50:50v/v) gradient flow rate at 1.0 mL/min for 30minutes. Samples was stored at 5°c temperature in sample cooler and Column oven temperature was maintained  in the method at 30°c  Respectively. The retention time of Thiotepa was 11.313 minutes. The proposed method was developed and validated with respect to specificity, accuracy, precision, linearity, Analyte Stability. Specificity of the Assay method shows no interference from Diluent and degrading products formed by alkaline, acidic, oxidative, Water Hydrolysis conditions. At Each level, %Recovery of Thiotepa in formulations was obtained to be in a range of 98-102%. The linearity of the assay was established in the range of 159.915-479.744µg/mL with correlation coefficient (R2) > 0.9999. This method was shows simple, precise, more accurate, stability indicating and reliable determination of Thiotepa for drug stability assay in pharmaceutical studies.

A simple, precise, novel stability-indicating method was developed and validated for the estimation of Bendamustine in pharmaceutical forms. The Assay method was developed by using a detector set at 235nm and reverse phase c18 column (Inertsil ODS-2,150mmx4.6mm, 5 μm).The mobile phase consisted of 0.1%Trifluoroacetic acid: Acetonitrile 70:30 (v/v) in isocratic flow rate at 1.5mL/min for 10minutes.Sample cooler temperature and Column oven temperature were monitored in the method at 5°c and 25°c Respectively. The retention time of bendamustine was 4.8min.The proposed method was achieved and validated with respect to precision, specificity, accuracy, linearity, range, Analyte Stability, Filter variability, Robustness. The %Recovery of Bendamustine at Each level in formulations was found to be in a range of 98-102%. The linearity of the assay was established in the range of 5.053 to 75.793 µg/mL with correlation coefficient (R2) > 0.9999. The limits of detection and quantification were 0.03 and 0.05mg/mL, respectively. Specificity of the assay demonstrates no interference from and degrading products formed by alkaline, acidic, oxidative, UV light and high temperature (Thermal) conditions. This method showed more accurate, rugged and reliable determination of Bendamustine for drug stability assay in pharmaceutical studies.