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Validation study of assay method for DX‐8951 and its metabolite in human plasma and urine by high‐performance liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry
Author(s) -
Oguma Toshihiro,
Konno Tomomi,
Inaba Atsuhiro,
Nakaoka Minoru
Publication year - 2001
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.44
Subject(s) - chromatography , chemistry , atmospheric pressure chemical ionization , tandem mass spectrometry , mass spectrometry , metabolite , liquid chromatography–mass spectrometry , high performance liquid chromatography , selected reaction monitoring , sample preparation , urine , chemical ionization , ionization , ion , biochemistry , organic chemistry
A new liquid chromatographic/mass spectrometric assay has been developed for the determination of DX‐8951, a new anti‐tumor drug, and its 4‐hydroxymethyl metabolite (UM‐1) in human plasma and urine. Solid‐phase extractions were used for sample preparation. A gradient reverse‐phase HPLC separation was developed with mobile phases consisting of trifluoroacetic acid and methanol. The detection was conducted using atmospheric pressure chemical ionization tandem mass spectrometry in the selected reaction monitoring mode. A structural analog, camptothecin (CPT), was used as the internal standard. The assay was validated for the determination of DX‐8951 and UM‐1 in human plasma and urine. The lower limits of quantitation of DX‐8951 and UM‐1 were 0.1 ng/mL in plasma and 1 ng/mL in urine. The method showed a satisfactory sensitivity, precision, accuracy, recovery and selectivity. Copyright © 2001 John Wiley & Sons, Ltd. Abbreviations used: CID Collision‐induced dissociationCPT camptothecinSRM selective reaction monitoringTFA trifluoro‐acetic acidUM‐1 4‐hydroxy methyl metabolite