Application of Elements of Quality by Design to Development and Optimization of HPLC Method for Fingolimod

Purpose: A HPLC method for Fingolimod was developed using a Quality by Design concept. QbD has gained importance in recent times due to regulatory requirements. Actual study started after determination of target profile and qualification instrument.
 Methods: Separation carried on Grace C-8 column (4.6 x 250 mm, 5-?m particle size).The composition mobile phase methanol 20 mM ammonium formate buffer pH5.8 gradient mode development is affected critical factors like pH, flow rate composition.
 Results: To the effects these three USP tailing, Box Behnken optimization model applied. Desirability set at Tailing less than 1.2.Analysis results done surface diagrams. Verification Software generated taking six replicates run. Thus optimised Finally validated as per ICH guideline.
 Conclusion: approach been successfully utilised bulk. All key aspect were tried be implemented said study.
 Systematic utilized which includes beginning with characteristics, instrument qualification, risk assessment, design experiment validation.
 Three i.e. Ph, concentration analysed their effect tailing responce. Interaction quadratic studied least possible runs model. Response diagrams contour plots coming conclusion are affecting response limits recorded. Optimum run condition obtained; Replicates having optimized taken confirm predicted actual response.