Development and validation of HPLC method for enantioseparation of Ibrutinib on immobilized chiral stationary phase

Novel HPLC method was developed for enantioresolution of tyrosine kinase inhibitor drug Ibrutinib (IBT). Separation and identification of IBT enantiomers was investigated using cellulose tris (3,5-dichlorophenylcarbamate) immobilized on silica gel (Chiral-pack-IC). Good baseline enantioseparation was achieved on Chiral-pack-IC under normal-phase condition composed of n-Hexane, ethanol in a ratio of 55 and 45 (%v/v) with 0.1% Diethyl amine and 0.3% Trifluoro acetic acid. Resolution between IBT and its enantiomer was above 4. The flow rate and column oven temperature were 0.9 mL/min and 30 °C respectively. Detection was carried out at 260 nm. Injection volume optimized was 10 µL. Developed method was validated in accordance with ICH guide lines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision, ruggedness and robustness.