AQbD-Based Development and Validation of HPTLC Method for Simultaneous Determination of Glycopyrronium, Formoterol Fumarate and Budesonide in Rotacaps.

Analytical quality by design was used to develop and validate a sensitive, accurate and precise high performance thin layer chromatography method for the determination of glycopyrronium (GLY), formoterol fumarate (FFD) and budesonide (BUD) in pharmaceutical dosage form (Rota caps). Design of Experiment was carried out by Placket-Burman screening design and Box- Behnken response surface methodology using peak area and Rf value as critical method attributes. Method operable design region was navigated for optimization and development of the method. The developed method was validated as per ICH Q2 guidelines. Linearity was found to be 0.25-1.25 μg/band, 0.12-0.60 μg/band and 4-20 μg/band respectively for GLY, FFD and BUD. Accuracy of the method was determined by recovery studies where the percentage recoveries were found to be 98-101%. The precision of the method was determined by repeatability and intermediate precision studies. The % RSD values were found to be less than 2, proving method was precise. The method was found specific and precise for the estimation of drugs. The developed method was applied for the assay of rotacaps and results were found in good agreement with the label claim.