Title: STABILITY INDICATING RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR DETERMINATION OF GEFITINIB IN BULK AS WELL AS IN PHARMACEUTICAL DOSAGE FORM BY USING PDA DETECTOR
Author(s): Ramesh Jayaprakash and Dr. Senthil Kumar Natesan
A simple, economic, accurate, sensitive, specific and precise stability indicating reverse phase high performance liquid chromatographic [RP- HPLC] method for the determination of Gefitinib in pure and tablet dosage form was developed and validated. The chromatographic separation was carried out using Shodex- C18 column [4.5 x 250 mm; 5 µm particle size] as a stationary phase, 0.02M potassium dihydrogen phosphate buffer [pH 6.5]: methanol: trifluro acetic acid [55:25:20 v/v/v] as a mobile phase, flow rate of 1 mL/min and the PDA detection was carried out at 254 nm. The retention time of Gefitinib was 3.247 minute. RP- HPLC method was developed with linearity range of 25-150 µg/mL of Gefitinib. The correlation coefficient [r2] was found to be 0.9999. The assay results obtained in good agreement with the corresponding labeled amount by developed method within range of 100.69 ± 0.4397. Accuracy of the method was confirmed by recovery studies and the recoveries were found to be between 99.86 % to 100.712 % and the corresponding %RSD was found to be 0.4057, precision, LOD, LOQ, specificity, robustness and ruggedness were met all the acceptance criteria for the validation of analytical method as per ICH Q2 (R1) guideline. This method can be conveniently used to detect the possible degradation product in the dosage form of Gefitinib during stability studies (acidic, alkaline, oxidative, thermal and photolytic). The method proved to be effective on application to a stressed marketed tablet formulation.
Keywords: Gefitinib; RP-HPLC; stability indicating method; validation; ICH-guidelines