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Imatinib assay by high‐performance liquid chromatography in tandem mass spectrometry with solid‐phase extraction in human plasma
Author(s) -
Moreno Jose María,
Wojnicz Aneta,
Steegman Juan Luis,
CanoAbad Maria F.,
RuizNuño Ana
Publication year - 2013
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.2819
Subject(s) - chemistry , chromatography , ammonium formate , electrospray ionization , solid phase extraction , mass spectrometry , calibration curve , tandem mass spectrometry , liquid chromatography–mass spectrometry , extraction (chemistry) , selected reaction monitoring , imatinib mesylate , detection limit , analytical chemistry (journal) , imatinib , myeloid leukemia , immunology , biology
We have developed a method of liquid chromatography in tandem with mass spectrometry to monitor therapeutic levels of imatinib in plasma, a selective inhibitor of protein tyrosine kinase. After solid‐phase extraction of plasma samples, imatinib and its internal standard, imatinib‐D8, were eluted with Zorbax SB‐C 18 at 60 °C, under isocratic conditions through a mobile phase consisting of 4 m m ammonium formate, pH: 3.2 (solution A) and acetonitrile solution B. The flow rate was 0.8 mL/min with 55% solution A + 45% solution B. Imatinib was detected and quantified by mass spectrometry with electrospray ionization operating in selected‐reaction monitoring mode. The calibration curve was linear in the range 10–5000 ng/mL, the lower limit of quantitation being 10 ng/mL. The method was validated according to the recommendations of the Food and Drug Administration, including tests of matrix effect (bias < 10%) and recovery efficiency (>80 and <120%). The method is precise (coefficient of variance intra‐day <2% and inter‐day <7%), accurate (95–108%), sensitive and specific. It is a simple method with very fast recording time (1.2 min) that is applicable to clinical practice. This will permit improvement of the pharmacological treatment of patients. Copyright © 2012 John Wiley & Sons, Ltd.