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Research Journal of Pharmacy and Technology
Year : 2018, Volume : 11, Issue : 8
First page : ( 3647) Last page : ( 3657)
Print ISSN : 0974-3618. Online ISSN : 0974-360X.
Article DOI : 10.5958/0974-360X.2018.00672.8

Separation, Identification and Quantification of process related Impurities and Stress Degradants of Gefitinib by LC-ESI-Q–TOF/MS

Kallepalli Pramadvara*, Annapurna Mukthinuthalapati Mathrusri

Department of Pharmaceutical Analysis and Quality Assurance, GITAM Institute of Pharmacy, GITAM University, Visakhapatnam-530045, India

*Corresponding Author E-mail: pramadvarakallepalli4@gmail.com

Online published on 31 October, 2018.

Abstract

Gefitinib, an anticancer drug and its process related impurities were estimated using WATERS 2695 Series HPLC system equipped with Quaternary gradient pumps and WATERS 2996 PDA detector with EMPOWER software. ESI-QTOF-MS system with Waters Quattro premier XE triple quadrupole with Acquity HPLC system with Masslynx software was used for the mass spectral studyof the impurities. Reverse phase C-18 column-Inertsil ODS 3V (150 X 4.6 mm, 5μm particle) was used and the total run time was 45 min. Gefitinib was subjected to forced degradation studies and the degradant products were analyzed using mass spectroscopy. Impurities (I -X) were separated on isocratic mode and calibrated using mass spectroscopy. Gefitinib was found to be more sensitive towards oxidation and three degradants were observed and their mass spectra also analyzed. The method was validated (ICH guidelines).

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Keywords

Gefitinib, RP-HPLC, ESI-QTOF-MS, stability indicating, Impurities, validation, ICH guidelines.

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