Drug Development and Validation of a Sensitive Bio-analytical LCMS/MS Method for Quantification of Asciminib-a Chronic Myeloid Leukemia Drug in Human Plasma

Author(s): Govindarao Yedlapalli* and Y. Ganesh Kumar


This study targeted to develop a reliable and less time consuming Liquid Chromatography–Mass Spectrometry/Mass spectrometry (LC–MS/MS) method for quantification of chronic myeloid leukemia drug, asciminib in human plasma using sunitinib as internal standard. The analyte asciminib and sunitinib were extracted from spiked plasma by adopting liquid-liquid extraction using methyl tertiary butyl ether solvent and chromatographed on an Alltima HP C18 (100 mm × 4.6 mm, 3 μm) column with pH 4.3 ammonium formate (5 mM) buffer and methanol in 45 (v/v):55 (v/v) at pH 4.3 mL/min at 1.0 mL/min flow in isocratic mode. The analysis completed within a total chromatographic run time of 4 min that facilitates less time and solvent consumption. The column separated analytes were recorded using mass detector with positive ion electrospray ionization source. The mass spectrum shows precursor-to-product ion transitions at m/z of 450/195 (m+1) for asciminib and 399/185 (m+1) for sunitinib. The method produces calibration curve linear in 2.5 ng/mL-200 ng/mL concentration range with sensitive detection limit of 0.075 ng/mL for asciminib. The mean plasma spiked extraction recoveries of both asciminib and internal standard was very high with acceptable % RSD in all precision studies. The analytes were noticed to be stable in a variety of stability studies performed. The method was validated to be sensitive, accurate and was suitable for determination of asciminib in human plasma and applicable for regular quality analysis studies.

image 10.4303/JDAR/236242

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