Determination of celecoxib in human plasma by liquid chromatography-tandem mass spectrometry.
A liquid chromatography-electrospray tandem mass spectrometry method was developed and validated to quantitate celecoxib in human plasma. The assay was based on protein precipitation with methanol and liquid chromatography on a C₁₈ column (55 mm × 2 mm, 3 μm), the mobile phase consisted of methanol-10 mM ammonium acetate (75:25, v/v). Quantification was performed by mass spectrometry in the multiple reaction monitoring mode with negative electrospray ionization at m/z 380→316 and 384→320 for celecoxib and the internal standard celecoxib-D₄, respectively. The lower limit of quantitation was 7.0 ng/ml using 0.1 ml of plasma and linearity was demonstrated up to 1800 ng/ml. Intra-assay and inter-assay precision expressed by relative standard deviation was less than 4% and inaccuracy did not exceed 6% at all levels. The assay was applied to the analysis of samples from a pharmacokinetic study.
Pharmakl s.r.o., Seydlerova 2451, CZ-15800 Prague 13, Czech Republic.
Pavel
P
Ptáček
Josef
J
Klíma
Jan
J
Macek
D000293:Adolescent; D000328:Adult; D000068579:Celecoxib; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D052246:Cyclooxygenase 2 Inhibitors / Q000097:blood*; D006801:Humans; D008297:Male; D008875:Middle Aged; D010949:Plasma / Q000737:chemistry*; D011720:Pyrazoles / Q000097:blood*; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D013449:Sulfonamides / Q000097:blood*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D055815:Young Adult
D052246:Cyclooxygenase 2 Inhibitors; D011720:Pyrazoles; D013449:Sulfonamides; D000068579:Celecoxib