Development & Validation of RP-HPLC Method for Quantitative Estimation of Dasatinib and its Impurities in Pharmaceutical Dosage Form

Abstract

Aim: The primary objective of the research work is to develop a effective, sensitive, economical and simple reverse phase HPLC method for the separation and quantification of Dasatinib and its impurities are described in tablet formulations. Study Design: HPLC based quantification studies. Place and Duration of Study: Department of Chemistry, Acharya Nagarjuna University, Guntur, Andhra Pradesh between April 2021 and August 2021. Methodology: Separation and quantification of Dasatinib and its impurities are done by using an Inertsil ODS-3V, 250 x 4.6 mm, 5µm and the mobile phase consists of two Channels A and B. Channel-A: pH 5.80 phosphate buffer : acetonitrile (90:10 v/v)   and Channel-B: acetonitrile : water (90:10 v/v). The flow rate is 1.0 ml/min. The column temperature was maintained at 25°C and sample temperature was maintained at 25°C, injection volume 10 µL and wavelength fixed at 320nm UV-detection. Results: There is no interference of diluent and placebo at Dasatinib and impurities peaks. The elution order and the retention times of impurities and Dasatinib obtained from individual standard preparations and mixed standard preparations are comparable. The limit of detection (LOD) and limit of quantitation (LOQ) for Dasatinib standard 0.147&0.048 µg/mL, impurity-A 0.334&0.110 µg/mL, impurity-C 0.184&0.061 µg/mL,  impurity-D 0.136&0.045 µg/mL, impurity-E 0.089&0.029 µg/mL  and impurity-F 0.222 & 0.073 µg/mL respectively. The linearity results for Dasatinib and all the impurities in the specified concentration range are found satisfactory, with a correlation coefficient greater than 0.99.Calibration curve was plotted and correlation co-efficient for Dasatinib and its impurities found to be 1.000, 0.9999, 0.9912, 1.000, 0.9932 and 0.9922 respectively. The accuracy studies were shown as % recovery for Dasatinib and its impurities at specification level. The limit of % recovered shown is in the range of 80 and 120% and the results obtained were found to be within the limits. Hence the method was found to be accurate. The method has validated as per ICH guidelines and all the validation parameters are satisfy the ICH Q2 specification acceptance limits Conclusion:  The developed LC method was validated with respect to specificity, precision, linearity, ruggedness and robustness. Therefore this method has high probability to adopt in pharmaceutical industry for regular analysis of Dasatinib tablet formulations.