Quantitative and selective assay of 5-methylindirubine, an inhibitor of cyclin-dependent kinases, in murine plasma using coupled liquid chromatography and electrospray tandem mass spectrometry

J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Sep 1;856(1-2):261-6. doi: 10.1016/j.jchromb.2007.06.006. Epub 2007 Jun 22.

Abstract

A sensitive and rapid LC-MS/MS assay for the quantitative determination of 5-methylindirubine (5-MI) in murine plasma is described. A 50-microL-murine plasma aliquot was spiked with an internal standard, indirubine-3-monoxime (IMO), and extracted with 1.25 mL diethyl ether. Dried extracts were reconstituted in methanol-water (8:2, v/v) and 10 microL-volumes were injected onto the HPLC system. Separation was achieved on a Gemini C18 column (150 mm x 2.1 mm ID, particle size 5 microm) using an alkaline eluent (10 mM ammonium hydroxide-methanol (5:95, v/v)). Detection was performed by negative ion electrospray followed by tandem mass spectrometry. The assay quantifies 5-MI in a range from 1 to 500 ng/mL using 50 microL of murine EDTA plasma samples. Validation results demonstrate that 5-MI concentrations can be accurately and precisely quantified in murine plasma. This assay is used to support pre-clinical pharmacologic studies with 5-MI.

Publication types

  • Validation Study

MeSH terms

  • Animals
  • Chromatography, High Pressure Liquid / methods*
  • Cyclin-Dependent Kinases / antagonists & inhibitors*
  • Indoles / blood*
  • Mice
  • Protein Kinase Inhibitors / blood*
  • Reference Standards
  • Sensitivity and Specificity
  • Spectrometry, Mass, Electrospray Ionization / methods*
  • Tandem Mass Spectrometry / methods*

Substances

  • 5-methylindirubine
  • Indoles
  • Protein Kinase Inhibitors
  • Cyclin-Dependent Kinases