Development and validation of liquid chromatography method for determination of Ibrutinib in finished dosage forms using quality by design approach
Naresh Konduru, Rambabu Gundla, Thirupathi Dongala, Naresh Kumar Katari, Ravindra Mallavarapu
Abstract
Abstract A simple, precise, linear, robust, accurate, and stability‐indicating liquid chromatography method was developed and validated to determine Ibrutinib in finished solid dosage forms by reversed‐phase high‐performance liquid chromatography/photodiode array detector. Separation was achieved using a Luna C18 150 mm × 4.6 mm × 3.0 μm with a suitable mobile phase. The mobile phase: A consists of a 10 mM phosphate buffer concentration and 1 mL triethylamine, adjusted to pH 5.6 with a diluted orthophosphoric acid solution and acetonitrile in the ratio of 95:5 v/v to enhance the results. Moreover, mobile phase ‐ B contains 85% of acetonitrile. The optimized chromatographic conditions such as flow rate 1.0 mL/min, injection volume 10 μL, column temperature 40°C, and wavelength 258 nm. The proposed method is significant because it was developed by the Quality by Design approach. All impurities were identified, such as degradation and placebo impurities without interference at principle peak retention time. After development, it has been validated as per current regulatory guidelines. Obtained recovery between 98 and 102% at 50–200% level; linearity found ( r 2 ) = 0.9999 from 20 to 200% level; precision results achieved <2.0% relative standard deviation; and the robustness study results are found satisfactory. It's beneficial.