title: Validation of liquid chromatography and liquid chromatography/tandem mass spectrometry methods for the determination of etoricoxib in pharmaceutical formulations.
abstract: Reversed-phase liquid chromatography (LC) and LC/tandem mass spectrometry (LC/MS/MS) methods were developed and validated for the determination of etoricoxib in pharmaceutical dosage forms. The LC method was performed by reversed-phase chromatography on a Synergi fusion C18 column (150 x 4.6 mm id) maintained at ambient temperature. The mobile phase consisted of 0.01 M phosphoric acid, pH 3.0-acetonitrile (62 + 38, v/v) at a flow rate of 1.0 mL/min, and photodiode array detection at 234 nm was used. The chromatographic separation was obtained within 7.0 min, and calibration curves were linear in the concentration range of 0.02-150 microg/mL. The LC/MS/MS method was performed on a Luna C18 column (50 x 3.0 mm id). The mobile phase consisted of acetonitrile-water (95 + 5)-0.1% acetic acid (90 + 10, v/v). Detection was performed by positive electrospray ionization in the multiple reaction monitoring mode, monitoring the transitions 359.3 > 280.0 and 332.0 > 95.0 for etoricoxib and piroxicam (internal standard), respectively. The chromatographic separation was obtained within 2.0 min, and calibration curves were linear in the concentration range of 1-5000 ng/mL. Validation parameters, such as specificity, linearity, precision, accuracy, and robustness, were evaluated, which gave results within the acceptable range for both methods. Moreover, the proposed methods were successfully applied for routine quality control analysis of pharmaceutical products and showed significant correlation (r = 0.9999) of the results.
authors.affiliation: Federal University of Santa Maria, Health Science Center, Postgraduate Program in Pharmaceutical Sciences, Santa Maria, Brazil.
authors.forename: Liberato
authors.initials: L
authors.lastname: Brum
authors.forename: Marcio
authors.initials: M
authors.lastname: Fronza
authors.forename: Danieli Catia
authors.initials: DC
authors.lastname: Ceni
authors.forename: Thiago
authors.initials: T
authors.lastname: Barth
authors.forename: Sergio Luiz
authors.initials: SL
authors.lastname: Dalmora
mesh_terms: D002626:Chemistry, Pharmaceutical; D002853:Chromatography, Liquid / Q000379:methods* / Q000592:standards / Q000706:statistics & numerical data; D016861:Cyclooxygenase Inhibitors / Q000032:analysis*; D000077613:Etoricoxib; D013058:Mass Spectrometry / Q000379:methods* / Q000592:standards / Q000706:statistics & numerical data; D011725:Pyridines / Q000032:analysis*; D011786:Quality Control; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods / Q000592:standards / Q000706:statistics & numerical data; D013450:Sulfones / Q000032:analysis*; D013607:Tablets
chemical_list: D016861:Cyclooxygenase Inhibitors; D011725:Pyridines; D013450:Sulfones; D013607:Tablets; D000077613:Etoricoxib