A STUDY OF ANALYTICAL METHOD DEVELOPMENT, VALIDATION AND FORCED DEGRADATION FOR SIMULTANEOUS ESTIMATION OF GLYCOPYRROLATE AND FORMOTEROL FUMARATE IN BULK DRUG BY UHPLC METHOD

摘要

The present study was proposed to develop a simple, rapid, and economical UHPLC method was described for the method development, validation and forced degradation for the simultaneous estimation of glycopyrrolate and formoterol fumarate in bulk drug. The chromatographic conditions were observed in the column using Zorbax RXC18 (150 × 4.6 mm) 5 μm using a mobile phase composition of Water: Acetonitrile: Methanol (20:30:50 v/v) and pH was adjusted to 3.0 with dilute orthophosphoric acid. The flow rate was 1.0 ml/min, and the analytes were recorded at 279 nm. The Retention time (RT) was observed in 1.208 for Glycopyrrolate and 5.897 for Formoterol fumarate. A calibration curve was linear with a coefficient correlation between 0.999 to 1.0 over a concentration range of 20-60μg/ml for glycopyrrolate and formoterol fumarate. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.003,0.011μg/ml for Glycopyrrolate and 0.108,0.32μg/ml for formoterol fumarate. All the validation parameters were within the acceptance range according to ICH norms. The validation and forced degradation study was performed for the proposed method and applied successfully to simultaneously estimate glycopyrrolate and formoterol fumarate. This method was precise, accurate, robust and economical.