QbD-Driven Approach to Cleaning Method Development and Validation for Darunavir Analysis in Oral Films.

Abstract

The current investigations involve developing a high-performance liquid chromatographic method that’s simple to operate, fast to establish, accurate, precise, and economical through design-enabled methods. A positive experimental design is offered to utilize the central composite design of pH and the mobile phase, two crucial components of the RP-HPLC technology. The chromatographic conditions were optimized with the release of Design Expert software version 13.0. Symmetry C18 column (4.6×150mm, 5µm) was used in the procedure, along with acetonitrile (20:80 v/v) and potassium dihydrogen orthophosphate buffer pH 4.0 as the mobile phase. There was a 0.70 ml/min flow rate. 263 nm is the wavelength of detection. Darunavir’s sharp, resolved peak was seen 2.3 minutes after swabbed samples from the 10*10 cm SS plate were injected. A linear calibration curve with an R2 of 0.9991 was observed in the concentration range of 0.25 to 25µg/ml. For precision %RSD is 1.03,1.48. Accuracy % concentration 50%,100%,150% mean recovery 99.43-100.53.LOD & LOQ 1.12µg/ml, 3.39µg/ml. Robustness was tested with modest modifications to the wavelength and flow rate. Forced degradation studies were carried out and found to be within the limits. the degradation parameters such as Acid, Base, Oxidative, Photolytic, and thermal degradation parameters are according to the ICH guidelines. % Assay was done for oral films and it was found to be within the limits. Thus, the outcomes unequivocally demonstrated that the QbD technique could be effectively used to enhance the HPLC method for the measurement of darunavir in production settings.