Use of pH and kinetic isotope effects to establish chemistry as rate-limiting in oxidation of a peptide substrate by LSD1

Biochemistry. 2009 Jun 16;48(23):5440-5. doi: 10.1021/bi900499w.

Abstract

The mechanism of oxidation of a peptide substrate by the flavoprotein lysine-specific demethylase (LSD1) has been examined using the effects of pH and isotopic substitution on steady-state and rapid-reaction kinetic parameters. The substrate contained the 21 N-terminal residues of histone H3, with a dimethylated lysyl residue at position 4. At pH 7.5, the rate constant for flavin reduction, k(red), equals k(cat), establishing the reductive half-reaction as rate-limiting at physiological pH. Deuteration of the lysyl methyls results in identical kinetic isotope effects of 3.1 +/- 0.2 on the k(red), k(cat), and k(cat)/K(m) values for the peptide, establishing C-H bond cleavage as rate-limiting with this substrate. No intermediates between oxidized and reduced flavin can be detected by stopped-flow spectroscopy, consistent with the expectation for a direct hydride transfer mechanism. The k(cat)/K(m) value for the peptide is bell-shaped, consistent with a requirement that the nitrogen at the site of oxidation be uncharged and that at least one of the other lysyl residues be charged for catalysis. The (D)(k(cat)/K(m)) value for the peptide is pH-independent, suggesting that the observed value is the intrinsic deuterium kinetic isotope effect for oxidation of this substrate.

Publication types

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

MeSH terms

  • Binding Sites
  • Deuterium / chemistry
  • Histone Demethylases
  • Humans
  • Hydrogen-Ion Concentration
  • Isotopes / chemistry
  • Kinetics
  • Oxidation-Reduction
  • Oxidoreductases, N-Demethylating / chemistry*
  • Oxidoreductases, N-Demethylating / metabolism
  • Peptides / chemistry
  • Peptides / metabolism
  • Structure-Activity Relationship
  • Substrate Specificity

Substances

  • Isotopes
  • Peptides
  • Deuterium
  • Histone Demethylases
  • KDM1A protein, human
  • Oxidoreductases, N-Demethylating