Assay of TNP-470 and Its Two Major Metabolites in Human Plasma by High-Performance Liquid Chromatography-Mass Spectrometry

In this study, a sensitive, specific assay for the determination of TNP-470 and its two major metabolites M-IV (also know as AGM-1883) and M-II in human plasma is reported. The assay involves liquid-liquid extraction of acidified plasma followed by reversedphase high-performance liquid chromatograph...

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Bibliographic Details
Published in:Journal of chromatographic science 2002-04, Vol.40 (4), p.214-218
Main Authors: Whalen, Carl T., Hanson, Glenn D., Putzer, Kathy J., Mayer, Michael D., Mulford, Darcy J.
Format: Article
Language:English
Subjects:
Analysis
Antibiotics, Antineoplastic - blood
Biological and medical sciences
Chromatography, High Pressure Liquid - methods
Cyclohexanes
General pharmacology
Humans
Mass Spectrometry - methods
Medical sciences
O-(Chloroacetylcarbamoyl)fumagillol
Pharmacology. Drug treatments
Reference Standards
Sensitivity and Specificity
Sesquiterpenes - blood
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Summary:In this study, a sensitive, specific assay for the determination of TNP-470 and its two major metabolites M-IV (also know as AGM-1883) and M-II in human plasma is reported. The assay involves liquid-liquid extraction of acidified plasma followed by reversedphase high-performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry. A liquid-liquid extraction using an organic solvent mixture (methyl-tert-butyl-ether-hexane, 1:1, v/v) is used in place of solid-phase extraction because it provides consistent recoveries for all analytes, including the internal standard. Retention times for the analytes and internal standard are less than 7 min. Within- and between-day precision is ≤ 6.5% and ≤ 13.3% relative standard deviation, respectively, for the three analytes. The lower limits of quantitation are 0.25, 0.5, and 1.0 ng/mL for TNP-470, M-IV, and M-II, respectively.
ISSN:0021-9665
1945-239X
DOI:10.1093/chromsci/40.4.214