Stability Indicating RP-HPLC Assay Method Development and ...

Available online at www.ijpras.comTable4.1 Method PrecisionSampleTable 4.2 System Precision% Assay1 100.992 101.733 101.154 100.005 101.426 101.73Mean 101.17SD 0.65%RSD 0.64Injection No.Area1 20967152 20979393 20955104 20958695 2099092MEAN 2097025SD 1486.23RSD 0.07Table 5. Recovery Analysis of DeferasiroxAccuracy:Accuracy of the method was determined bycalculating recoveries of Deferasirox by method ofstandard addition. The mean recoveries found to be101.86%. for Deferasirox (Table 4). The highrecovery values indicate that the method isaccurate.Selectivity:Selectivity of the method was demonstrated afterobserving that the excipients did not produceabsorption peaks in the chromatogram and did notinterfere with the exact determination of theanalytes in the accuracy assay in addition,chromatograms were completely super imposablewith those recorded by simultaneous detection at245 nm, all of which served as indication that thedetermination was not interfered by any of theingredients.Forced DegradationNo degradation was observed during UV exposure.Degradation was observed in acidic, basic andperoxide conditions. The table 6 indicates thedegradation condition and peak purity data.Robustness:The robustness of the proposed method wasexamined against small, deliberate variations ofcritical parameters such as the composition of themobile phase, flow rate and column temperature.Robustness indicates that small and deliberatechanges were not significantly affecting thedetermination so method was found to be robust.The detail data of robustness study is shown intable 7.Table 7. Data for RobustnessAccuracyLevelAmountAddedAmt.Recovered%Recovery50% 25.30 25.85 102.250% 25.40 25.98 102.3100% 50.30 50.55 100.5100% 50.60 50.49 99.8150% 75.40 77.52 102.8150% 75.20 77.73 103.4MEAN : 101.86 %SD : 0.32RSD : 0.32ParameterMobile phasecompositionFlow rate (inml/min.)STATISTICALPARAMETERS% ASSAY48:52 101.1752:48 101.170.9 101.271.1 101.31MEAN 101.25SD 1.1%RSD 0.96Stability of Analytical Solution:The sample and standard preparations were storedat room temperature and tested against freshlyprepared standard preparation for 24 hours. Theassay results are within the limit. Results are shownin table 8.43