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Determination of triamcinolone in human plasma by a sensitive HPLC-ESI-MS/MS method: application for a pharmacokinetic study using nasal spray formulation

César, Isabela Costa, Byrro, Ricardo Martins Duarte, de Santana e Silva Cardoso, Fabiana Fernandes, Mundim, Iram Moreira, de Souza Teixeira, Leonardo, de Sousa, Weidson Carlo, Gomes, Sandro Antônio, Bellorio, Karini Bruno, Brêtas, Juliana Machado, Pianetti, Gerson Antônio
Journal of mass spectrometry 2011 v.46 no.3 pp. 320-326
acetonitrile, ammonium acetate, betamethasone, humans, ionization, monitoring, nose, pH, pharmacokinetics, sampling, tandem mass spectrometry, triamcinolone, volunteers
A liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS) method for the quantitation of triamcinolone in human plasma after nasal spray application was developed and validated. Betamethasone was used as internal standard (IS). The analytes were extracted by a liquid-liquid procedure and separated on a Zorbax Eclipse XDB C₁₈ column with a mobile phase composed of 2 mM aqueous ammonium acetate pH 3.2 and acetonitrile (55:45). Selected reaction monitoring was performed using the transitions m/z 435 → 415 and m/z 393 → 373 to quantify triamcinolone acetonide and betamethasone, respectively. Calibration curve was constructed over the range of 20-2000 pg/ml for triamcinolone acetonide. The lower limit of quantitation was 20 pg/ml. The mean RSD values were 4.6% and 5.7% for the intra-run and inter-run precision, respectively. The mean accuracy value was 98.5% and a recovery rate corresponding to 97.5% was achieved. No matrix effect was detected in the samples. The validated method was successfully applied to determine the plasma concentrations of triamcinolone acetonide in healthy volunteers, in a pharmacokinetic study with nasal spray formulation.