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Validation of stability indicating rp-hplc method for the assay of ibrutinib in pharmaceutical dosage form

Sureshbabu Kapavarapu, Ramu Golkonda3, Rambabu Chintala

A stability indicating RP-HPLC method was developed and validated as per international chemical harmonization guidelines, and adopted for the assay of Ibrutinib in bulk and tablet dosage forms. The chromatographic separation was carried out by using Waters (Alliance) HPLC 2695 series system equipped with UV-Visible spectrophotometer as detector. Mobile phase composed of 0.1% Orthophosphoric acid buffer and acetonitrile in the ratio 70:30%v/vwas allowed to flowthrough InertsilODS 100mmx 4.6 mm, 5m column at a flow rate of 0.8ml/minute, maintaining the column temperature at 30°C. About 20µl of standard or sample solution was injected into the column and the components were detected at a wavelength of 320nm. Systemprecision and method precision of the proposed method was evaluated as %RSD and found to be 1.7252 and 1.0583 respectively. Accuracy of the developed method as percent of mean recovery at three different concentrations 50, 100 and 150% with respect to target concentration was determined and found to be 100.68, 100.90 and 100.33 respectively. The peak area was found to be proportional to concentration of Ibrutinib within the linearity limits 3.5-21.0µg/ml, slope, intercept and correlation coefficient were determined by linear regression analysis. The developed method was found to be robust and rugged and was applied for quality control analysis of pharmaceutical formulations. The stability of the drug under different degradation conditions was examined and found to be stable. The proposed method was found to be simple and suggested for an alternative method in quality control in any quality control laboratories.