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

 
: Klawitter, J.; Zhang, Y.L.; Klawitter, J.; Anderson, N.; Serkova, N.J.; Christians, U.

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Biomedical chromatography : BMC 23 (2009), No.12, pp.1251-1258
ISSN: 0269-3879
ISSN: 1099-0801
English
Journal Article
Fraunhofer ITEM ()

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.

: http://publica.fraunhofer.de/documents/N-113387.html