Published:Journal of Chromatographic Science,
ISSN 0021-9665Volume
41, Number 1, January 2003, pp. 44-49
Automated Solid-Phase Extraction Method for the Determination
of Piperaquine in Plasma by Peak Compression Liquid Chromatography
N. Lindegårdh[1],[3], M. Ashton[2], and Y. Bergqvist[1],[3]
[1]Dalarna University College, 781 88 Borlänge, Sweden;
[2]Department
of Pharmacology, Sahlgrenska Academy at Gothenburg University, 405 30 Gothenburg,
Sweden; and
[3]Department of Analytical Chemistry, Uppsala University, 751 21 Uppsala,
Sweden
A validated bioanalytical method for the determination of piperaquine (PQ)
in plasma by solid-phase extraction (SPE) and liquid chromatography (LC) using
peak compression is presented. Protein is precipitated from plasma with acetonitrile–1%
aqueous acetic acid (85:15, v/v). An internal standard (IS) is added to the
samples before they are loaded onto a strong cation exchanger (Isolute PRS)
SPE column. PQ and the IS are analyzed by LC on a Zorbax SB-CN column (250 ¥ 4.0
mm) with the mobile phase acetonitrile–phosphate buffer [I = 0.1, pH
2.5 (12:88, v/v)] and UV detection at 345 nm. Trichloroacetic acid (TCA) is
added to the samples prior to injection into the chromatography system. PQ
elutes in a gradient of TCA, which enables peak compression of PQ and significantly
higher peak efficiency as a result. The intraassay precision for plasma is
determined to be 5.4% at 3.00µM and 5.8% at 0.050µM. The interassay
precision for plasma is 1.3% at 3.00µM and 10.0% at 0.050µM. The
lower limit of quantitation and the limit of detection are 0.025 and 0.005µM,
respectively.
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