Validation of an isocratic HPLC method to detect 2-fluoro-beta-alanine for the analysis of dihydropyrimidine dehydrogenase activity

J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Jul 1;878(21):1889-92. doi: 10.1016/j.jchromb.2010.05.010. Epub 2010 May 19.

Abstract

The efficacy of the chemotherapeutic drug 5'-fluorouracil is reduced by catabolism to 2'-fluoro-beta-alanine (FBAL), a three-step reaction in which dihydropyrimidine dehydrogenase (DPD) catalyzes the rate-limiting step. To study in vitro DPD activity, we developed and validated an isocratic, reverse-phase HPLC method to detect and quantify FBAL without using multiple columns or radiolabeled substrates. Pre-column derivatization of FBAL was performed using o-phthalaldehyde in the presence of two sulfur donors, ethanthiol or beta-mercaptoethanol, and the resulting products assayed. Calibration curves were linear over a range of 10-200 microg/ml and the method was successfully applied to the examination of DPD activity in cultured cells.

Publication types

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

MeSH terms

  • Cell Line, Tumor
  • Chromatography, High Pressure Liquid / methods*
  • Chromatography, Reverse-Phase
  • Dihydrouracil Dehydrogenase (NADP) / metabolism*
  • Drug Stability
  • Fluorouracil
  • Humans
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Sulfhydryl Compounds / chemistry
  • beta-Alanine / analogs & derivatives*
  • beta-Alanine / analysis
  • beta-Alanine / chemistry
  • beta-Alanine / metabolism
  • o-Phthalaldehyde / chemistry

Substances

  • Sulfhydryl Compounds
  • beta-Alanine
  • alpha-fluoro-beta-alanine
  • o-Phthalaldehyde
  • Dihydrouracil Dehydrogenase (NADP)
  • ethanethiol
  • Fluorouracil