A sensitive method for the quantification of fluticasone propionate in human plasma by high-performance liquid chromatography/atmospheric pressure chemical ionisation mass spectrometry
| Autor: | Kenneth F. Brown, J. P. Seale, Bruce N. Tattam, Yuan Nian (Benny) Li |
|---|---|
| Rok vydání: | 1997 |
| Předmět: |
Chemical ionization
Chromatography Clinical Biochemistry Extraction (chemistry) Anti-Inflammatory Agents Analytical chemistry Reproducibility of Results Pharmaceutical Science Atmospheric-pressure chemical ionization Reversed-phase chromatography Mass spectrometry High-performance liquid chromatography Mass Spectrometry Analytical Chemistry Androstadienes Acetic anhydride chemistry.chemical_compound chemistry Calibration Drug Discovery Fluticasone Humans Solid phase extraction Chromatography High Pressure Liquid Spectroscopy |
| Zdroj: | Journal of Pharmaceutical and Biomedical Analysis. 16:447-452 |
| ISSN: | 0731-7085 |
| Popis: | A highly sensitive and selective method has been developed for the quantification of fluticasone propionate (FP) in human plasma. The drug was isolated from human plasma using C 18 solid-phase extraction cartridges. The analysis was based on high-performance liquid chromatography/atmospheric pressure chemical ionisation mass spectrometry (HPLC/APCI/MS), using the 22R epimer of budesonide (BUD) acetate, synthesised using acetic anhydride, as internal standard. The mass spectrometer was operated in APCI mode with selected ions at tune masses of 473.2 and 501.2 m / z , corresponding to the MH + of acetylated (22R)BUD and FP, respectively. The mobile phase used was a mixture of 50% ethanol in water with a flow rate of 0.45 ml min −1 . The system was optimised by tuning the capillary and tube lens with a concentrated solution of FP. The recovery of FP from human plasma was 86.3%. Linearity of response was obtained over the concentration range 0.2–4.0 ng ml −1 . The intra-assay and inter-assay variability were 6.3 and 2.9%, respectively. The lower limit of quantification was 0.2 ng ml −1 when a solid-phase extraction preceded the HPLC/APCI/MS. |
| Databáze: | OpenAIRE |
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