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

• Published in: Journal of mass spectrometry. 2011-03, Vol.46 (3), p.320-326
• Main Authors: 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
• Format: Article
• Language: English
• Subjects: Analysis; Betamethasone; Biological and medical sciences; Chromatography, High Pressure Liquid - methods; Eclipses; Formulations; General pharmacology; HPLC-ESI-MS/MS; Human; Humans; Ionization; Linear Models; Liquids; Mass spectrometry; Medical sciences; nasal spray; Nasal Sprays; pharmacokinetics; Pharmacology. Drug treatments; plasma; Reproducibility of Results; Sensitivity and Specificity; Spectrometry, Mass, Electrospray Ionization - methods; Sprayers; Sprays; Tandem Mass Spectrometry - methods; triamcinolone; Triamcinolone - administration & dosage; Triamcinolone - blood; Triamcinolone - pharmacokinetics
• ISSN: 1076-5174; 1096-9888; 1096-9888
• DOI: 10.1002/jms.1896

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. Copyright © 2011 John Wiley & Sons, Ltd.