Title
The determination of budesonide and fluticasone in human sputum samples collected from COPD patients using LC-MS/MS
Author
Buscher, B.A.P.
Jägfeldt, H.
Sandman, H.
Brust-van Schaik, R.
van Schaik, F.
Brüll, L.P.
Publication year
2012
Abstract
A bioanalytical method for the quantitative determination of budesonide and fluticasone in human sputum was developed. Sputolysin ® Reagent was added to the sputum samples. After incubation (37°C; 60-70min under shaking) and automated solid phase extraction the extracts were analysed using LC-MS/MS. Budesonide and fluticasone showed good linearity (r>0.99) over the range 0.1-100nM in the first and second validation batch, and over the range 0.25-10,000nM in the third and fourth validation batch. The lower limit of quantification (LLOQ) achieved was 5nM for budesonide and fluticasone in 100μL human sputum. Intra-run and inter-run RSD for four quality control levels (5-100nM) were within 6.9% (budesonide) and 8.0% (fluticasone). The accuracy ranged from -11.4% to -1.6% (budesonide), and from -11.8% to 0.4% (fluticasone). The validated method was applied to clinical sputum samples from COPD patients. © 2011 Elsevier B.V.
Subject
Life Triskelion BV
QS - Quality & Safety TAP - Toxicology and Applied Pharmacology
EELS - Earth, Environmental and Life Sciences TNO Bedrijven
Biology
Healthy Living
Bioanalysis
HPLC
Mass spectrometry
Sample pre-treatment
Sputum
Validation
To reference this document use:
http://resolver.tudelft.nl/uuid:e74e055a-87c6-43cd-b55a-42d1db6d2e8c
DOI
https://doi.org/10.1016/j.jchromb.2011.10.029
TNO identifier
445988
ISSN
1570-0232
Source
Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences, 880 (1), 6-11
Document type
article