Abstract

METHOD DEVELOPMENT AND VALIDATION OF IBRUTINIB BY RP HPLC IN BULK AND PHARMACEUTICAL DOSAGE FORM.

Vykuntam Uppala, Ayesha Tabassum*, Lavanya K., Neeraja V., JVC Sharma

ABSTRACT

A simple, Precised, Accurate method was developed for the estimation of Ibrutinib by RP-HPLC technique. Chromatographic conditions used are stationary phase Kromosil150mm x 4.6 mm, 5, Mobile phase0.1% OPA: Acetonitrile in the ratio of 40:60and flow rate was maintained at 1ml/min, detection wave length was 296nm, column temperature was set to 30oC and diluent was mobile phase Conditions were finalized as optimized method. System suitability parameters were studied by injecting the standard six times and results were well under the acceptance criteria. Linearity study was carried out between 25% to150 % levels, R2 value was found to be as 0.999. Precision was found to be 1.01 for repeatability and 1.50 for intermediate precision. LOD and LOQ are 0.394μg/ml and 1.194μg/ml respectively. By using above method assay of marketed formulation was carried out 100.55% was present. Degradation studies of ibrutinib were done, in all conditions purity threshold was more than purity angle and within the acceptable range.

Keywords: HPLC, Ibrutinib, Method development. ICH Guidelines.