Bioanalytical method development and alidation of ibrutinib in biological matrices by LC-MS/MS
- Vol. 2(3)
- M P Innovare Academic Sciences Pvt Ltd 2019
- 22-26p.
Objective: The main aim of the research was to develop a fast and highly sensitive bioanalytical LC- MS/MS technique for the quantitation of ibrutinib in human plasma . Method s: Chromatography has achieved on a reverse phase -symmetry C , A. ASHOK KUMAR Mewar University, Chittorgarh, Rajasthan, India Emai l: jessie.hepsebah@gmail.com 18 (75 mm × 4.6 mm, 3.5 μm) column with gradient elution by acetonitrile, methanol and 0.1 % v/v formic acid as the mobile phase. Chromatographic peaks were resolved with 0.7 m l/min flow rate . Drug was extracted with ethyl acetate solvent by liquid -liquid extraction method. Monitoring of transition of m/z 441.2 and 55. 01 for ibrutinib and 446.5 and 60.01 for Ibrutinib -D5 were made on multiple reaction monitoring. Result s: Calibration curve of ibrutinib was linear over 1 -600 ng/ml concentration range with a regression coefficient (r 2 Keyword s: Ibrutinib , Chronic lymphocytic leukemia, LC -MS/MS, FDA guidelines and Dilution integrity ) value of >0.99 . The % RSD values were less than 8.5% for inter -day and intra -day precision and accuracy. The method has excellent recovery and the percentage recovery values of lower quality control (LQC) , median quality control ( MQC ) and higher quality control ( HQC ) samples were 101.86%, 102.8% , and 99.28 % respectively . Conclusio n: The drug was stable for more time at variable stability conditions and method was successfully applicable to the regular analysis of ibrutinib in biological matrices