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    Simultaneous determination of primaquine and carboxyprimaquine in plasma using solid phase extraction and LC-MS assay

    Access Status
    Fulltext not available
    Authors
    Page-Sharp, Madhu
    Ilett, K.
    Betuela, I.
    Davis, T.
    Batty, Kevin
    Date
    2012
    Type
    Journal Article
    
    Metadata
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    Citation
    Page-Sharp, Madhu and Ilett, Kenneth F. and Betuela, Inoni and Davis, Timothy M.E. and Batty, Kevin T. 2012. Simultaneous determination of primaquine and carboxyprimaquine in plasma using solid phase extraction and LC-MS assay. Journal of Chromatography B. 902: pp. 142-146.
    Source Title
    Journal of Chromatography B
    DOI
    10.1016/j.jchromb.2012.06.019
    ISSN
    1570-0232
    URI
    http://hdl.handle.net/20.500.11937/40766
    Collection
    • Curtin Research Publications
    Abstract

    Sensitive bioanalytical methods are required for pharmacokinetic studies in children, due to the small volume and modest number of samples that can be obtained. We sought to develop a LC–MS assay for primaquine and its active metabolite, carboxyprimaquine, following simultaneous, solid phase extraction of both analytes from human plasma. The analysis was conducted on a single-quad LC–MS system (Shimadzu Model 2020) in ESI+ mode, with quantitation by selected ion monitoring. Primaquine, carboxyprimaquine and 8-aminoquinoline (internal standard) were separated using a mobile phase of 80:20 methanol:water with 0.1% (v/v) formic acid and a Luna C18 HPLC column, at ambient temperature. Solid phase extraction of the analytes from plasma (0.5 mL) was achieved with Oasis® HLB cartridges. The retention times for primaquine, 8-aminoquinoline and carboxyprimaquine were 3.3, 5.7 and 8.5 min, respectively. The calibration curve range (2–1500 μg/L) was appropriate for the limits of quantification and detection for primaquine (2 μg/L and 1 μg/L, respectively) and carboxyprimaquine (2.5 μg/L and 1 μg/L) and the anticipated plasma concentrations of the analytes. Intra- and inter-day precision for both primaquine and carboxyprimaquine was <10% across the concentration range 5–1000 μg/L. Accuracy for both analytes was <15% (5–500 μg/L). This validated LC–MS method with solid phase extraction facilitates the simultaneous analysis of primaquine and carboxyprimaquine from small volumes of human plasma, with run time <10 min, recovery >85% and sensitivity of 1–2 μg/L.

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