Identification of Degradant Impurity in Gefitinib by Using Validated RRLC Method


Degradation pathway for gefitinib is established as per ICH recommendations by validated and stability indicating reverse phase liquid chromatographic method. Gefitinib is subjected to stress conditions of acid, base, oxidation, thermal and photolysis. Significant degradation is observed in acid and base stress conditions. Two impurities are studied among which one impurity is found prominent degradant. The stress samples are assayed against a qualified reference standard and the mass balance is found close to 99.5%. Efficient chromatographic separation is achieved on a Agilent make XDB-C18, 50 × 4.6 mm with 1.8 μm particles stationary phase with simple mobile phase combination delivered in gradient mode and quantification is carried at 250 nm at a flow rate of 0.5 mL·min. In the developed RPLC method the resolution between gefitinib and the potential impurities is found to be greater than 5.0. Regression analysis shows an r value (correlation coefficient) of greater than 0.998 for gefitinib and the two potential impurities. This method is capable to detect the impurities of gefitinib at a level of 0.01% with respect to test concentration of 0.5 mg·mL for a 4-μL injection volume. The developed RRLC method is validated with respect to specificity, linearity & range, accuracy, precision and robustness for impurities determination and assay determination.

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@inproceedings{Venkataramanna2011IdentificationOD, title={Identification of Degradant Impurity in Gefitinib by Using Validated RRLC Method}, author={Madireddy Venkataramanna and Indukuri Venkata Somaraju and Kondra Sudhakar Babu}, year={2011} }