Article ID | Journal | Published Year | Pages | File Type |
---|---|---|---|---|
1217035 | Journal of Chromatography B | 2012 | 4 Pages |
A quantitative bioanalytical liquid chromatography–tandem mass spectrometric (LC–MS/MS) assay for the JAK2 inhibitor CYT387 was developed and validated. Plasma samples were pre-treated using protein precipitation with acetonitrile containing cediranib as internal standard. The extract was directly injected into the chromatographic system after dilution with water. This system consisted of a sub-2 μm particle, trifunctional bonded octadecyl silica column with a gradient using 0.005% (v/v) of formic acid in a mixture of water and methanol. The eluate was transferred into the electrospray interface with positive ionization and the analyte was detected in the selected reaction monitoring mode of a triple quadrupole mass spectrometer. The assay was validated in a 0.25–1000 ng/ml calibration range. Within day precisions were 3.0–13.5%, between day precisions 5.7% and 14.5%. Accuracies were between 96% and 113% for the whole calibration range. The drug was stable under all relevant analytical conditions. Finally, the assay was successfully used to assess drug levels in mice.
► The first bioanalytical assay for CYT387 has been reported. ► The LC–MS/MS assay is simple, fast and sensitive. ► The assay has successfully been validated in the 0.25–1000 ng/ml range. ► The drug is stable under all conditions relevant for the assay.