A cellular system for quantitation of vitamin K cycle activity: structure-activity effects on vitamin K antagonism by warfarin metabolites

Blood. 2014 Jan 23;123(4):582-9. doi: 10.1182/blood-2013-05-505123. Epub 2013 Dec 2.

Abstract

Warfarin and other 4-hydroxycoumarins inhibit vitamin K epoxide reductase (VKOR) by depleting reduced vitamin K that is required for posttranslational modification of vitamin K-dependent clotting factors. In vitro prediction of the in vivo potency of vitamin K antagonists is complicated by the complex multicomponent nature of the vitamin K cycle. Here we describe a sensitive assay that enables quantitative analysis of γ-glutamyl carboxylation and its antagonism in live cells. We engineered a human embryonic kidney (HEK) 293-derived cell line (HEK 293-C3) to express a chimeric protein (F9CH) comprising the Gla domain of factor IX fused to the transmembrane and cytoplasmic regions of proline-rich Gla protein 2. Maximal γ-glutamyl carboxylation of F9CH required vitamin K supplementation, and was dose-dependently inhibited by racemic warfarin at a physiologically relevant concentration. Cellular γ-glutamyl carboxylation also exhibited differential VKOR inhibition by warfarin enantiomers (S > R) consistent with their in vivo potencies. We further analyzed the structure-activity relationship for inhibition of γ-glutamyl carboxylation by warfarin metabolites, observing tolerance to phenolic substitution at the C-5 and especially C-6, but not C-7 or C-8, positions on the 4-hydroxycoumarin nucleus. After correction for in vivo concentration and protein binding, 10-hydroxywarfarin and warfarin alcohols were predicted to be the most potent inhibitory metabolites in vivo.

Publication types

  • Research Support, N.I.H., Extramural

MeSH terms

  • Alcohols / chemistry
  • Anticoagulants / chemistry
  • Doxycycline / chemistry
  • Factor IX / chemistry
  • Flow Cytometry
  • HEK293 Cells
  • Humans
  • Inhibitory Concentration 50
  • Liver / metabolism
  • Phenol / chemistry
  • Protein Binding
  • Protein Structure, Tertiary
  • Stereoisomerism
  • Structure-Activity Relationship
  • Vitamin K / antagonists & inhibitors*
  • Vitamin K / chemistry
  • Vitamin K / metabolism*
  • Vitamin K Epoxide Reductases / antagonists & inhibitors
  • Vitamin K Epoxide Reductases / metabolism
  • Warfarin / analogs & derivatives
  • Warfarin / chemistry*

Substances

  • Alcohols
  • Anticoagulants
  • Vitamin K
  • Phenol
  • Warfarin
  • 10-hydroxywarfarin
  • Factor IX
  • Vitamin K Epoxide Reductases
  • Doxycycline