Development and validation of a sensitive assay for the quantification of imatinib using LC/LC-MS/MS in human whole blood and cell culture

Biomed Chromatogr. 2009 Dec;23(12):1251-8. doi: 10.1002/bmc.1247.

Abstract

We developed and validated a semi-automated LC/LC-MS/MS assay for the quantification of imatinib in human whole blood and leukemia cells. After protein precipitation, samples were injected into the HPLC system and trapped onto the enrichment column (flow 5 mL/min); extracts were back-flushed onto the analytical column. Ion transitions [M + H](+) of imatinib (m/z = 494.3 --> 394.3) and its internal standard trazodone (372.5 --> 176.3) were monitored. The range of reliable response was 0.03-75 ng/mL. The inter-day precisions were: 8.4% (0.03 ng/mL), 7.2% (0.1 ng/mL), 6.5% (1 ng/mL), 8.2% (10 ng/mL) and 4.3% (75 ng/mL) with no interference from ion suppression. Autosampler stability was 24 hs and samples were stable over three freeze-thaw cycles. This semi-automated method is simple with only one manual step, uses a commercially available internal standard, and has proven to be robust in larger studies.

Publication types

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

MeSH terms

  • Antineoplastic Agents / blood*
  • Benzamides
  • Cell Line, Tumor
  • Chromatography, High Pressure Liquid / methods*
  • Humans
  • Imatinib Mesylate
  • Limit of Detection
  • Piperazines / blood*
  • Pyrimidines / blood*
  • Reference Standards
  • Reproducibility of Results
  • Tandem Mass Spectrometry / methods*

Substances

  • Antineoplastic Agents
  • Benzamides
  • Piperazines
  • Pyrimidines
  • Imatinib Mesylate