Automated solid-phase extraction method for the determination of piperaquine in plasma by peak compression liquid chromatography.

• 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.

Ämnesord

NATURVETENSKAP  -- Kemi -- Analytisk kemi (hsv//swe)

NATURAL SCIENCES  -- Chemical Sciences -- Analytical Chemistry (hsv//eng)

MEDICIN OCH HÄLSOVETENSKAP  -- Medicinska och farmaceutiska grundvetenskaper -- Farmaceutiska vetenskaper (hsv//swe)

MEDICAL AND HEALTH SCIENCES  -- Basic Medicine -- Pharmaceutical Sciences (hsv//eng)

Nyckelord

Antimalarials

analysis

Calibration

Chromatography

Liquid

methods

Humans

Hydrogen-Ion Concentration

Quinolines

blood

Reference Standards

Reproducibility of Results

Sensitivity and Specificity

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