title: Automated solid-phase extraction method for the determination of piperaquine in plasma by peak compression liquid chromatography.
abstract: 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 x 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 3.00 microM and 5.8% at 0.050 microM. The interassay precision for plasma is 1.3% at 3.00 microM and 10.0% at 0.050 microM. The lower limit of quantitation and the limit of detection are 0.025 and 0.005 microM, respectively.
authors.affiliation: Dalarna University College, 781 88 Borlänge, Sweden.
authors.forename: N
authors.initials: N
authors.lastname: Lindegårdh
authors.forename: M
authors.initials: M
authors.lastname: Ashton
authors.forename: Y
authors.initials: Y
authors.lastname: Bergqvist
mesh_terms: D000962:Antimalarials / Q000032:analysis*; D002138:Calibration; D002853:Chromatography, Liquid / Q000379:methods*; D006801:Humans; D006863:Hydrogen-Ion Concentration; D011804:Quinolines / Q000097:blood*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D010879:Piperazines
chemical_list: D000962:Antimalarials; D011804:Quinolines; C034759:piperaquine; D010879:Piperazines