Gas chromatograph–mass spectrometric method for the determination of carvedilol and its metabolites in human urine
A sensitive and efficient method was developed for the determination of carvedilol and its metabolites in human urine by gas chromatography–mass spectrometry (GC–MS). Urine samples were hydrolyzed with β-glucuronidase/arylsulfatase (from Helix pomatia) and the target compounds were extracted with li...
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Veröffentlicht in: | Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Analytical technologies in the biomedical and life sciences, 2005-08, Vol.822 (1), p.70-77 |
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Format: | Artikel |
Sprache: | eng |
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Zusammenfassung: | A sensitive and efficient method was developed for the determination of carvedilol and its metabolites in human urine by gas chromatography–mass spectrometry (GC–MS). Urine samples were hydrolyzed with β-glucuronidase/arylsulfatase (from
Helix pomatia) and the target compounds were extracted with liquid–liquid extraction. The extracts were completely derivatized with MSTFA and MBTFA and analyzed by GC–MS using an Ultra-2 column. The linearity of the assay ranges were 0.75–75
ng
mL
−1 for carvedilol and
o-desmethyl carvedilol (
o-DMC), and 3.0–75
ng
mL
−1 for 4-hydroxyphenyl carvedilol (4-HPC) and 5-hydroxyphenyl carvedilol (5-HPC). The absolute recovery of carvedilol and its metabolites added to a blank urine sample was 80.1–97.8%. The limits of detection (LOD) and quantitation (LOQ) of carvedilol and
o-DMC were 0.30 and 0.75
ng
mL
−1, and its of 4-HPC and 5-HPC were 0.75 and 3.0
ng
mL
−1, respectively. The reproducibilities were 1.86–11.5% for the intra-day assay, and 0.70–1.71% for the inter-day assay precision and the degree of inaccuracy was −3.0 to 3.9% at the concentration of 75
ng
mL
−1. The proposed GC–MS method was effective for the determination of carvedilol and its three metabolites in human urine. |
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ISSN: | 1570-0232 1873-376X |
DOI: | 10.1016/j.jchromb.2005.05.023 |