Determination of kynurnine and tryptophan, biomarkers of indoleamine 2,3-dioxygenase by LC-MS/MS in plasma and tumor

Bioanalysis. 2018 Aug 1;10(16):1335-1344. doi: 10.4155/bio-2018-0041. Epub 2018 Aug 21.

Abstract

Aim: Tryptophan (Trp) and kynurnine (Kyn) are a pair of biomarkers for indoleamine 2,3-dioxygenase which closely related to the tumor immune escape. To evaluate the effect of drugs on the indoleamine 2,3-dioxygenase activity, the specific and accurate LC-MS/MS methods were developed and validated for simultaneous determination Kyn and Trp in mouse plasma and tumor tissues using surrogate analytes Kyn-d4 and Trp-d5 calibrators.

Results: Plasma and tumor homogenates samples were pretreated with the solid phase extraction which assured the method having high recovery (>90% in plasma and >80% in tumor) and no matrix effect. The methods were validated for specificity, linearity, accuracy and precision, recovery, matrix effect and stability using surrogate analytes Kyn-d4 and Trp-d5 in authentic matrices.

Conclusion: The validated methods have been successfully applied to the pharmacodynamic study of INCB024360 in CT26 tumor bearing mice after single dose and multiple dosing.

Keywords: INCB024360; LC–MS/MS; indoleamine 2,3-dioxygenase; kynurenine; surrogate analytes; tryptophan.

MeSH terms

  • Animals
  • Biomarkers / blood
  • Biomarkers / metabolism
  • Blood Chemical Analysis / methods*
  • Chromatography, Liquid
  • Indoleamine-Pyrrole 2,3,-Dioxygenase / antagonists & inhibitors
  • Indoleamine-Pyrrole 2,3,-Dioxygenase / metabolism*
  • Kynurenine / blood*
  • Kynurenine / metabolism
  • Male
  • Mice
  • Mice, Inbred BALB C
  • Neoplasms / blood*
  • Tandem Mass Spectrometry
  • Tryptophan / blood*
  • Tryptophan / metabolism

Substances

  • Biomarkers
  • Indoleamine-Pyrrole 2,3,-Dioxygenase
  • Kynurenine
  • Tryptophan