Open AccessAnalytical Separation and Characterisation of Degradation Products and the Development and Validation of a Stability-Indicating Method for the Estimation of Impurities in Ipratropium Bromide Respules Formulation
Author(s) -
Anas Rasheed,
Osman Ahmed
Publication year - 2017
Publication title -
international journal of applied pharmaceutical sciences and research
Language(s) - English
Resource type - Journals
ISSN - 2455-8095
DOI - 10.21477/ijapsr.v2i3.8101
Subject(s) - ipratropium bromide , chemistry , impurity , chromatography , detection limit , bromide , degradation (telecommunications) , organic chemistry , computer science , medicine , telecommunications , asthma , bronchodilator
A short selective, precise, accurate and sensitive stability-indicating gradient LC-MS/MSn method was developed for the quantitative determination of process-related impurities and degradation products of Ipratropium bromide in pharmaceutical respules formulations. During the stress study, the degradation products of Ipratropium bromide were well-resolved from Ipratropium bromide and its impurities and the mass balances were found to be satisfactory in all the stress conditions, thus proving the stability-indicating capability of the method. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection and quantification, accuracy, precision, ruggedness, and robustness. During the stability analysis of the drug product, one unknown impurity was detected by the above stability-indicating method. The flow rate was 0.5 ml/min and effluent was monitored at 242nm. Retention time was found to be 5.0150.15 min. The LOD and LOQ values for were found to be 0.20996 (?g/ml) and 0.63624 (?g/ml) respectively.