Quantification of perifosine, an alkylphosphocholine anti-tumour agent, in plasma by pneumatically assisted electrospray tandem mass spectrometry coupled with high-performance liquid chromatography
article
An HPLC assay with tandem mass spectrometric detection in the positive-ion Turbo-Ion-Spray((TM)) (TISP) mode for the fast and sensitive determination of perifosine ((I), D-21266) in human plasma was developed, utilising the structural analogue, miltefosine ((II), D-18506), as internal standard. Automated solid-phase extraction of diluted plasma samples, based on 250-μl plasma aliquots, at pH 6.5, allowed a reliable quantification of perifosine down to 4 ng/ml. Injection of 200 μl of plasma extracts onto a 100x3 mm normal-phase analytical column at a flow-rate of 0.5 ml/min provided retention-times of 2.4 and 2.1 min for perifosine (I) and the internal standard (II), respectively. The standard curves were linear from 4 to 2000 ng/ml using weighted linear regression analysis (1/Y2). The inter-assay and intra-assay accuracies for the calibration standards were within +0.9% and -0.2%, exhibiting precisions (C.V.) of ±6.5 and ±7.3%, respectively. Up to 100 unknowns may be analysed each 24 h per analyst. Copyright (C) 1999 Elsevier Science B.V.
Topics
AlkylphosphocholinePerifosineAntineoplastic agentMiltefosinePerifosineUnclassified drugAccuracyAutomationCalibrationControlled studyDrug blood levelDrug determinationHigh performance liquid chromatographyHumanHuman experimentHuman tissueMass spectrometryOral drug administrationPriority journalSolid phase extractionTechniqueCalibrationChromatography, High Pressure LiquidHumansMass SpectrometryPhosphorylcholineQuality ControlSpectrometry, FluorescenceSpectrophotometry, Ultraviolet
TNO Identifier
234918
ISSN
13872273
Source
Journal of Chromatography B: Biomedical Sciences and Applications, 721(2), pp. 257-269.
Pages
257-269
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