HIGH-THROUGHPUT LIQUID CHROMATOGRAPHIC DETERMINATION OF ROFECOXIB IN HUMAN PLASMA USING A FULLY AUTOMATED ON-LINE SOLID-PHASE EXTRACTION SYSTEM

• Published in: Journal of liquid chromatography & related technologies Vol. 24; no. 6; pp. 799 - 812
• Main Authors: Hsieh, John Y.-K., Lin, Li, Matuszewski, Bogdan K.
• Format: Journal Article
• Language: English
• Published: Colchester Taylor & Francis Group 01.01.2001; Taylor & Francis
• Subjects: Analysis; Biological and medical sciences; General pharmacology; Medical sciences; Pharmacology. Drug treatments; rofecoxib; Solid phase extraction; Biological fluid; Prostaglandin-endoperoxide synthase; Chemical analysis; On line; Sulfone; Isozyme; HPLC chromatography; Selectivity; Photochemical reaction; Derivatization; Oxygen heterocycle; Postcolumn; Blood; Blood plasma; Sample preparation; Quantitative analysis; Human; Automation; Fluorescence detector; Enzyme; Coupled method; Oral administration; Enzyme inhibitor; Lactone; Non steroidal antiinflammatory agent; Benzenic compound; Oxidoreductases; Pharmacokinetics
• ISSN: 1082-6076; 1520-572X
• DOI: 10.1081/JLC-100103411

A fully automated on-line solid-phase extraction method combined with high-performance liquid chromatography-fluorescence detection for the determination of rofecoxib in human plasma is described. A Spark Holland PROSPEKT system was used to perform all the automated on-line sample extraction and quantitation tasks, including sample loading, cartridge conditioning and washing, analyte elution, and start of a data acquisition system. Under postcolumn ultraviolet-irradiation conditions, the analytes were photochemically converted to highly fluorescent products and then monitored by a fluorescence detector. The assay was validated in the concentration range of 0.5-100 ng/mL using 0.25 mL of human plasma. The utility of this method was demonstrated by analysis of plasma samples from human subjects receiving oral doses of rofecoxib. ‡ This work was presented at the Fifteenth Annual International Symposium on Laboratory Automation and Robotics, October 1997, Boston, MA, USA.