A rapid and sensitive HPLC-APCI-MS/MS method determination of fluticasone in human plasma: application for a
Ricardo Martins Duarte Byrro1, Isabela Costa César, Fabiana Fernandes de Santana e Silva Cardoso
1Instituto de Ciências Farmacêuticas, Alameda Coronel Eugênio Jardim 53, 74175-100 Goiânia, GO, Brazil. ricardobyrro@bol.com.br
Abstract:
A sensitive method for the determination of fluticasone in plasma was developed using high performance liquid chromatography with tandem mass spectrometric detection, whereas beclomethasone was used as internal standard. The analytes were extracted with a simple liquid-liquid extraction from the plasma samples and separated on an ACE C(18) 50 × 4.6 mm i.d.; 5 μm particle size column with a mobile phase consisting of acetonitrile - 0.01% formic acid (48:52, v/v) at a flow rate of 1 ml/min. Detection was achieved by an Applied Biosystems API 5000 mass spectrometer (LC-MS/MS) set at unit resolution in the multiple reaction monitoring mode. Atmospheric pressure chemical ionization (APCI) was used for ion production. The mean recovery for fluticasone propionate was 85%, with a lower limit of quantification set at 2 pg/mL. The validated analytical method was applied to a bioequivalence study of fluticasone propionate administered by nasal spray formulations in human volunteers.
