title: Development and validation of a reversed-phase liquid chromatographic method for separation and simultaneous determination of COX-2 inhibitors in pharmaceuticals and its application to biological fluids.
abstract: An isocratic reversed-phase high-performance liquid chromatographic method has been developed for separation and simultaneous determination of COX-2 inhibitors, viz., celecoxib, rofecoxib, valdecoxib, nimesulide and nabumetone, using 4-chloro-2-nitroaniline as internal standard. Good chromatographic separation was achieved using a reversed-phase Inertsil C(18) column with mobile phase consisting of methanol and 0.05% aqueous glacial acetic acid (68:32 v/v) using photodiode array (PDA) detector at 230 nm. It was validated with respect to accuracy, precision, linearity, limit of detection and quantification. The linearity range was found to be 1.0--20 microg/mL and the percentage recoveries were between 97.55 and 100.14. The method is suitable not only for the estimation of active ingredients in pharmaceutical dosage forms but also in vitro estimations in human plasma. It is simple, rapid, selective and capable of detecting and determining COX-2 inhibitors with a detection limit of 0.127--1.040 microg/mL simultaneously.
authors.affiliation: HPLC/UV Group, Division of Analytical Chemistry, Discovery Laboratory, Indian Institute of Chemical Technology, Hyderabad 50 0007, India. rnrao@ins.iictnet.com
authors.forename: R Nageswara
authors.initials: RN
authors.lastname: Rao
authors.forename: S
authors.initials: S
authors.lastname: Meena
authors.forename: D
authors.initials: D
authors.lastname: Nagaraju
authors.forename: A Raghu Ram
authors.initials: AR
authors.lastname: Rao
mesh_terms: D002074:Butanones / Q000097:blood; D000068579:Celecoxib; D002853:Chromatography, Liquid / Q000379:methods*; D052246:Cyclooxygenase 2 Inhibitors / Q000032:analysis* / Q000302:isolation & purification*; D006801:Humans; D007555:Isoxazoles / Q000097:blood; D007783:Lactones / Q000097:blood; D000077430:Nabumetone; D011720:Pyrazoles / Q000097:blood; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013449:Sulfonamides / Q000097:blood; D013450:Sulfones / Q000097:blood; D000096926:Benzenesulfonamides
chemical_list: D002074:Butanones; D000068579:Celecoxib; D052246:Cyclooxygenase 2 Inhibitors; D007555:Isoxazoles; D007783:Lactones; D000077430:Nabumetone; D011720:Pyrazoles; D013449:Sulfonamides; D013450:Sulfones; C116926:rofecoxib; C406224:valdecoxib; D000096926:Benzenesulfonamides; C012655:nimesulide