1. DEVELOPMENT OF A LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY METHOD FOR THE DETERMINATION OF INDIRUBIN-5-NITRO-3′-MONOXIME, A NOVEL CDK INHIBITOR, IN RAT PLASMA.
- Author
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Kim, HyunMi, Kim, Yong-Chul, Kim, JaeIl, Choi, YongSeok, and Kim, YoonGyoon
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LIQUID chromatography-mass spectrometry , *TANDEM mass spectrometry , *INDIRUBIN , *PHARMACOKINETICS , *CYCLIN-dependent kinase inhibitors , *BLOOD plasma , *LABORATORY rats - Abstract
A simple and rapid liquid chromatography-tandem mass spectrometry (LC–MS/MS) method has been developed and validated for the quantitation of indirubin-5-nitro-3′-monoxime (5-NIO) in rat plasma using 5-chloro-5′-chloro-indirubinoxime as the internal standard. The sample preparation involved protein precipitation using acetonitrile. Separation was achieved on an Xterra column C18 (2.1 mm × 50 mm, i.d. 5 µm) using a mixture of 0.1% formic acid-water/acetonitrile (18:82, v/v) as the mobile phase at a flow rate of 300 µL/min. Quantitation was performed on a triple quadrupole mass spectrometer employing electrospray ionization and multiple reaction monitoring (MRM) in negative ion mode. The total chromatographic run time was 2.5 min, and the calibration curves of 5-NIO were linear (correlation coefficient range: 0.9989–0.9999) over the concentration range of 0.2–2000 ng/mL in rat plasma. Also, the detection limit of the method was 0.05 ng/mL and it showed good accuracy and precision within the concentration range of 0.45–376 ng/mL. This validated method was successfully applied to estimating the pharmacokinetic parameters of 5-NIO following intravenous administration of 5-NIO to rats. [ABSTRACT FROM AUTHOR]
- Published
- 2012
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