title: Simple and sensitive method for the determination of celecoxib in human serum by high-performance liquid chromatography with fluorescence detection.
abstract: A simple method is described for the determination of the cyclooxygenase-2 specific inhibitor celecoxib in human serum by HPLC using the demethylated analogue as internal standard. After protein precipitation with acetonitrile, samples were extracted with chloroform. Separation was achieved on a Prontosil C18 AQ column (150x3 mm I.D., 3-microm particle size) at a flow-rate of 0.35 ml/min using water-acetonitrile (40:60, v/v) as the mobile phase. Using fluorescence detection with excitation at 240 nm and emission at 380 nm, the limit of quantification was 12.5 ng/ml for a sample size of 0.5 ml of serum. The assay was linear in the concentration range of 12.5-1500 ng/ml and showed good accuracy and reproducibility. At all concentrations intra- and inter-assay variabilities were below 11% with less than 9% error. The method was applied to the determination of celecoxib for pharmacokinetic studies in man.
authors.affiliation: Dr. Margarete Fischer-Bosch-Institut für Klinische Pharmakologie, Stuttgart, Germany.
authors.forename: Frank
authors.initials: F
authors.lastname: Schönberger
authors.forename: Georg
authors.initials: G
authors.lastname: Heinkele
authors.forename: Thomas E
authors.initials: TE
authors.lastname: Mürdter
authors.forename: Stefanie
authors.initials: S
authors.lastname: Brenner
authors.forename: Ulrich
authors.initials: U
authors.lastname: Klotz
authors.forename: Ute
authors.initials: U
authors.lastname: Hofmann
mesh_terms: D000328:Adult; D000368:Aged; D000068579:Celecoxib; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D016861:Cyclooxygenase Inhibitors / Q000097:blood* / Q000493:pharmacokinetics; D006801:Humans; D011720:Pyrazoles; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013050:Spectrometry, Fluorescence; D013449:Sulfonamides / Q000097:blood* / Q000493:pharmacokinetics
chemical_list: D016861:Cyclooxygenase Inhibitors; D011720:Pyrazoles; D013449:Sulfonamides; D000068579:Celecoxib