Enantioselective determination of ibuprofen in plasma by high-performance liquid chromatography-electrospray mass spectrometry.
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) NH(4)OH 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 microg/ml and the linear range was 0.12-90.0 microg/ml for both enantiomers. The method proved to be suitable for single dose pharmacokinetic studies.
Bonato
Pierina Sueli
PS
Faculdade de Ciências Farmacêuticas de Ribeirão Preto, Universidade de São Paulo, Avenida do Café S/N, 14040-903 Ribeirão Preto-SP, Brazil. psbonato@fcfrp.usp.br
Del Lama
Maria Perpetua F M
MP
de Carvalho
Roberto
R
D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000097:blood*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006801:Humans; D007052:Ibuprofen / Q000097:blood*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013237:Stereoisomerism
D000894:Anti-Inflammatory Agents, Non-Steroidal; D007052:Ibuprofen