Abstract
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 was started after determination of target profile and qualification of instrument.
 Methods: Separation was carried on a Grace C-8 column (4.6 x 250 mm, 5-μm particle size).The composition of mobile phase was methanol and 20 mM ammonium formate buffer of pH5.8 in gradient mode HPLC method development is affected by critical factors like pH, flow rate and mobile phase composition.
 Results: To study the effects of these three factors on USP tailing, Box Behnken optimization model was applied. Desirability of the model was set at Tailing less than 1.2.Analysis of results was done using surface diagrams. Verification of Software generated results was done by taking six replicates of the run. Thus developed and optimised method was Finally validated as per ICH guideline.
 Conclusion: A Quality by Design approach has been successfully utilised in method development of the Fingolimod in bulk. All key aspect of QbD were tried to be implemented in said study.
 Systematic approach was utilized for method development which includes beginning with determination of target profile characteristics, instrument qualification, risk assessment, design of experiment and validation.
 Three factors i.e. Ph, flow rate and methanol concentration were analysed for their effect on USP tailing as a responce. Interaction and quadratic effect of the factors were studied with least possible runs by using Box Behnken model. Response surface diagrams and contour plots were studied for coming to conclusion which factors are affecting response and their limits were recorded. Optimum run condition was obtained; Replicates of run having optimized condition were taken to confirm the predicted response with actual response.
Highlights
Systematic approach was utilized for method development which includes beginning with determination of target profile characteristics, instrument qualification, risk assessment, design of experiment and validation
Fingolimod [Trade name: Gilenya, Novartis (FTY720),; 2-amino-2-[2-(4-octylphenyl) ethyl]1,3-propanediol] is a recently discovered molecule approved by the United States Food and Drug Administration (USFDA) for treating multiple sclerosis [1]
“Quality by design (QbD) is systematic approach to development that begins with predefined objectives and emphasizes product and process understanding and process control based on sound science and quality risk management” (ICH guidelines, 2012).QbD has gained importance in recent times due to regulatory requirements
Summary
Fingolimod [Trade name: Gilenya, Novartis (FTY720),; 2-amino-2-[2-(4-octylphenyl) ethyl]1,3-propanediol] is a recently discovered molecule approved by the United States Food and Drug Administration (USFDA) for treating multiple sclerosis [1]. Fingolimod (FTY720) is a oral immunomodulating agent which preventslymphocyte recirculation from lymphoid organs [2]. Fingolimod primarily decrease the entry of T lymphocytes from secondary lymphoid organs, thereby inhibiting neuroinflammation [3]. “QbD is systematic approach to development that begins with predefined objectives and emphasizes product and process understanding and process control based on sound science and quality risk management” (ICH guidelines, 2012).QbD has gained importance in recent times due to regulatory requirements. USFDA has accelerated QbD drive to encourage the risk based approach and thorough understanding of processes which is going to help the regulatory bodies in review process. The main aspect in QbD is that quality is ‘built inby understanding the effect of the various system parameters.Effects are analysed for their influence on quality of product that is desired which supports in establishing the design space which is defined as the “multidimensional combination and interaction of input variables that have been demonstrated to provide assurance of quality” [4]
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