Method Development And Validation Of An Lc–Esi-Ms/Ms Technique For The Quantitation Of Fedratinib In Biological Matrices

Abstract

An LC–ESI-MS/MS technique for the quantitation of anticancer agent fedratinib in plasma samples was developed and subjected for validation. Internal standard for the evaluation of drug was ledipasvir. After the extraction process from 200 μL plasma by liquid liquid extraction technique, samples were isolated on a Zorbax SB(250mm x 4.6mm, 5µm) C₁₈ column with 0.1%V/V formic acid and acetonitrile in the ratio of 10:90 as mobile phase with 0.80 mL/min infusion flow rate. Total time for elution of analytes was 3.5 min. The technique was subjected for the validation in accordance with FDA standard guidelines in the concentration level of 1.5–5000.00 ng/mL for fedratinib with correlation coefficient value of 0.9994. The intra day and inter day precision findings were within 4.32% and the assay accuracy was 95.31–104.06 % of the nominal values. Matrix   factor   ranges   from 94.25– 104.85 % with a %CV of 4.61 for analyte at LQC level and at HQC level, the matrix   factor range was 94.62–103.88%  with  a  %CV  of  4.02. Stabilities revealed that the method has high degree of stability. The developed method can be applied successfully to routine analysis in quality control, bioavailability and bioequivalence studies of biological samples.