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Enantioselective determination of ibuprofen in plasma by high-performance liquid chromatography–electrospray mass spectrometry

2003; Elsevier BV; Volume: 796; Issue: 2 Linguagem: Inglês

10.1016/j.jchromb.2003.08.031

1873-376X

Pierina Sueli Bonato, Maria Perpétua F.M. Del Lama, Roberto de Carvalho,

Microfluidic and Capillary Electrophoresis Applications

The enantioselective analysis of ibuprofen (IBU), a chiral nonsteroidal anti-inflammatory drug, in human plasma was carried out by high-performance liquid chromatography (HPLC)–mass spectrometry (LC–MS–MS). The plasma samples were prepared by liquid–liquid extraction using hexane:ethyl acetate (8:2, v/v). The HPLC chiral resolution of IBU was obtained using a chiral stationary phase based on a tris-(3,5-dimethylphenylcarbamate) amylose derivative, under reversed phase conditions (CHIRALPAK AD-RH column), using a mobile phase consisting of methanol:water (8:2, v/v), containing 0.1% of an aqueous solution of phosphoric acid at pH 2, at a flow rate of 0.6 ml/min. A make-up liquid of 4.5% (w/v) NH4OH aqueous solution was used to assure optimum electrospray ionization in the negative mode. The coefficients of variation and deviation from nominal values were lower than 15% for both within- and between-day assays. The quantitation limit was 0.12 μg/ml and the linear range was 0.12–90.0 μg/ml for both enantiomers. The method proved to be suitable for single dose pharmacokinetic studies.