ANALYTICAL SEPARATION AND CHARACTERISATION OF DEGRADATION PRODUCTS METHOD FOR THE ESTIMATION OF IMPURITIES IN FLUOROMETHOLONE IN PARENTERAL DOSAGE FORM

Mohd Shafi*, Dr. Osman Ahmed and Dr. Anas Rasheed

ABSTRACT

A short selective, precise, accurate and sensitive LC-MS/MSn method was developed for the quantitative determination of process-related impurities and degradation products of Fluorometholone in pharmaceutical parenteral dosage formulations. During the study, the degradation products of Fluorometholone were well-resolved from Fluorometholone and its impurities and the mass balances were found to be satisfactory in all the stress conditions, thus proving 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, three unknown impurities were detected by the above method. The flow rate was 1.5 ml/min and effluent was monitored at 240nm. Retention time was found to be 5.205±0.012 min. The LOD and LOQ values for were found to be 0.3245 (μg/ml) and 0.983 (μg/ml)respectively.

Keywords: Fluorometholone, LC-MS/MSn, Validation, stability indicating method, degradation products.