Development and validation of a bioanalytical method using automated solid-phase extraction and LC-UV for the simultaneous determination of lumefantrine and its desbutyl metabolite in plasma

Document identifier: oai:dalea.du.se:1202
Access full text here:10.1016/j.jpba.2004.07.041
Keyword: Engineering and Technology, Chemical Engineering, Teknik och teknologier, Kemiteknik, Antimalarial; lumefantrine; lipophilic; liquid chromatography; solid-phase extraction; stability; validation
Publication year: 2005
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SDG 3 Good health and wellbeing
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Abstract:

A bioanalytical method for the determination of lumefantrine (LF) and its metabolite desbutyl-lumefantrine (DLF) in plasma by solid-phase extraction (SPE) and liquid chromatography has been developed. Plasma proteins were precipitated with acetonitrile: acetic acid (99:1, v/v) containing a DLF analogue internal standard before being loaded onto a octylsilica (3 M Empore) SPE column. Two different DLF analogues were evaluated as internal standards. The compounds were analysed by liquid chromatography UV detection on a SB-CN (250 mm x 4.6 mm) column with a mobile phase containing acetonitrile-sodium phosphate buffer pH (2.0; 0.1 M) (55:45, v/v) and sodium perchlorate 0.05 M. Different SPE columns were evaluated during method development to optimise reproducibility and recovery for LF, DLF and the two different DLF analogues. The within-day precisions for LF were 6.6 and 2.1% at 0.042 and 8.02 μ g/mL, respectively, and for DLF 4.5 and 1.5% at 0.039 and 0.777 μ g/mL, respectively. The between-day precisions for LF were 12.0 and 2.9% at 0.042 and 8.02 μ g/mL, respectively, while for DLF 0.7 and 1.2% at 0.039 and 0.777 μ g/mL, respectively. The limit of quantification was 0.024 and 0.021 μ g/mL for LF and DLF, respectively. Different amounts of lipids in plasma did not affect the absolute recovery of LF or DLF.

Authors

Niklas Lindegårdh

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A. Annerberg

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Daniel Blessborn

Högskolan Dalarna; Kemiteknik
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Yngve Bergqvist

Högskolan Dalarna; Kemiteknik
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N. Day

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N.J. White

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