Derivatization of the tricarboxylic acid intermediates with O-benzylhydroxylamine for liquid chromatography-tandem mass spectrometry detection

Anal Biochem. 2014 Nov 15:465:134-47. doi: 10.1016/j.ab.2014.07.027. Epub 2014 Aug 4.

Abstract

The tricarboxylic acid (TCA) cycle is an interface among glycolysis, lipid metabolism, and amino acid metabolism. Increasing interest in cancer metabolism has created a demand for rapid and sensitive methods for quantifying the TCA cycle intermediates and related organic acids. We have developed a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to quantify the TCA cycle intermediates in a 96-well format after O-benzylhydroxylamine (O-BHA) derivatization under aqueous conditions. This method was validated for quantitation of all common TCA cycle intermediates with good sensitivity, including α-ketoglutarate, malate, fumarate, succinate, 2-hydroxyglutarate, citrate, oxaloacetate, pyruvate, isocitrate, and lactate using a 8-min run time in cancer cells and tissues. The method was used to detect and quantify changes in metabolite levels in cancer cells and tumor tissues treated with a pharmacological inhibitor of nicotinamide phosphoribosyl transferase (NAMPT). This method is rapid, sensitive, and reproducible, and it can be used to assess metabolic changes in cancer cells and tumor samples.

Keywords: Derivatization; LC–MS/MS; O-benzylhydroxylamine; Tricarboxylic acid cycle intermediates.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Cell Line, Tumor
  • Chromatography, Liquid
  • Citric Acid Cycle*
  • Cytokines / antagonists & inhibitors
  • Cytokines / metabolism
  • Enzyme Inhibitors / pharmacology
  • Humans
  • Hydroxylamines / chemistry*
  • Mass Spectrometry / methods*
  • Neoplasm Proteins / antagonists & inhibitors
  • Neoplasm Proteins / metabolism
  • Neoplasms / metabolism*
  • Neoplasms / pathology
  • Nicotinamide Phosphoribosyltransferase / antagonists & inhibitors
  • Nicotinamide Phosphoribosyltransferase / metabolism
  • Tricarboxylic Acids / analysis
  • Tricarboxylic Acids / chemistry
  • Tricarboxylic Acids / metabolism*

Substances

  • Cytokines
  • Enzyme Inhibitors
  • Hydroxylamines
  • Neoplasm Proteins
  • Tricarboxylic Acids
  • benzyloxyamine
  • Nicotinamide Phosphoribosyltransferase
  • nicotinamide phosphoribosyltransferase, human