title: Development and Validation of a UPLC Method by the QbD-Approach for the Estimation of Rabeprazole and Levosulpiride from Capsules.
abstract: Statistical experimental design was used to optimize the chromatographic separations of two pharmaceutical compounds from their respective potential impurities. A fractional factorial design was utilized to study the effects of pH, organic solvent in mobile phases A&B, and flow rate on the resolution of Rabeprazole and Rabeprazole Sulfone, which had closely eluting peaks. A desirability function applied to the optimized conditions predicted the peak resolution between 2.2 and 2.7 for the Rabeprazole & Rabeprazole Sulfone impurity. The chromatographic method employed an Acquity UPLC, BEH C18 column (100 × 2.1 mm i.d., 1.7 μm particle size) with the mobile phase consisting of a phosphate buffer, pH 6.5, and acetonitrile in a gradient program. The flow rate and injection volumes were 0.45 mL/min & 5 μl, respectively, and detection was done at 254 nm. The chromatographic method was validated for linearity, accuracy, precision, specificity, and ruggedness according to ICH guidelines. The results clearly showed that the quality by design concept could be effectively applied to optimize a UPLC chromatographic method with fewer trials and error-free experimentation.
authors: Analytical Research and Development, Integrated Product Development, Dr. Reddy's Laboratories Ltd., Bachupally, Hyderabad-500 072, India.
authors: Veera Raghava Raju
authors: VR
authors: Thummala
authors: Analytical Research and Development, Integrated Product Development, Dr. Reddy's Laboratories Ltd., Bachupally, Hyderabad-500 072, India.
authors: Raja Kumar
authors: RK
authors: Seshadri
authors: Analytical Research and Development, Integrated Product Development, Dr. Reddy's Laboratories Ltd., Bachupally, Hyderabad-500 072, India.
authors: Satya Sankarsana Jagan Mohan
authors: SS
authors: Tharlapu
authors: School of Chemistry, Andhra University, Visakhapatnam-530003, A.P., India.
authors: Mrutyunjaya Rao
authors: MR
authors: Ivaturi
authors: School of Chemistry, Andhra University, Visakhapatnam-530003, A.P., India.
authors: Someswara Rao
authors: SR
authors: Nittala
keywords: Experimental design; Levosulpiride; Method Validation; Rabeprazole sodium; UPLC