Article ID Journal Published Year Pages File Type
1217035 Journal of Chromatography B 2012 4 Pages PDF
Abstract

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.

Related Topics
Physical Sciences and Engineering Chemistry Analytical Chemistry
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