A LC-MS/MS method for the analysis of intracellular nucleoside triphosphate levels

Pharm Res. 2009 Jun;26(6):1504-15. doi: 10.1007/s11095-009-9863-9. Epub 2009 Mar 17.

Abstract

Purpose: To simultaneously quantify intracellular nucleoside triphosphate (NTP) and deoxynucleoside triphosphate (dNTP) pools and to assess their changes produced by interfering with ribonucleotide reductase (RNR) expression in leukemia cells.

Methods: A HPLC-MS/MS system was used to quantify intracellular NTP and dNTP pools.

Results: The assay was linear between 50 nM, the lower limit of quantification (LLOQ), and 10 muM in cell lysate. The within-day coefficients of variation (CVs, n = 5) were found to be 12.0-18.0% at the LLOQ and 3.0-9.0% between 500 and 5,000 nM for dNTPs and 8.0-15.0% and 2.0-6.0% for NTPs. The between-day CVs (n = 5) were 9.0-13.0% and 3.0-11.0% for dNTPs and 9.0-13.0% and 3.0-6.0% for NTPs. The within-day accuracy values were 93.0-119.0% for both NTPs and dNTPs. ATP overlapped with dGTP and they were analyzed as a composite. This method was applied to measure basal intracellular dNTPs/NTPs in five leukemia cell lines exposed to the RNR antisense GTI-2040. Following drug treatment, dCTP and dATP levels were found to decrease significantly in MV4-11 and K562 cells. Additionally, perturbation of dNTP/NTP levels in bone marrow sample of a patient treated with GTI-2040 was detected.

Conclusions: This method provides a practical tool to measure intracellular dNTP/NTP levels in cells and clinical samples.

Publication types

  • Research Support, N.I.H., Extramural
  • Research Support, Non-U.S. Gov't
  • Validation Study

MeSH terms

  • Antimetabolites, Antineoplastic / therapeutic use
  • Bone Marrow Cells / drug effects
  • Bone Marrow Cells / metabolism
  • Cell Line, Tumor
  • Chromatography, Liquid / methods*
  • Cytarabine / therapeutic use
  • Humans
  • Leukemia / metabolism*
  • Leukemia / therapy*
  • Leukemia, Myeloid, Acute / metabolism*
  • Leukemia, Myeloid, Acute / therapy*
  • Linear Models
  • Nucleotides / analysis*
  • Nucleotides / isolation & purification
  • Oligodeoxyribonucleotides / therapeutic use
  • Sensitivity and Specificity
  • Tandem Mass Spectrometry / methods*

Substances

  • Antimetabolites, Antineoplastic
  • Nucleotides
  • Oligodeoxyribonucleotides
  • Cytarabine
  • GTI2040