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Simultaneous determination of unlabeled and carbon-13-labeled etoricoxib, a new cyclooxygenase-2 inhibitor, in human plasma using HPLC-MS/MS.
Rose, M J; Agrawal, N; Woolf, E J; Matuszewski, B K.
Afiliación
  • Rose MJ; Merck Research Laboratories, Department of Drug Metabolism, West Point, Pennsylvania 19486, USA. mark_rose@merck.com
J Pharm Sci ; 91(2): 405-16, 2002 Feb.
Article en En | MEDLINE | ID: mdl-11835200
A method for the simultaneous determination of etoricoxib and its carbon-13 analog ((13)C(6)-etoricoxib) from human plasma has been developed and used to support bioavailability studies. Plasma samples (0.5 mL) were extracted by using a 3M Empore 96-well plate (C(8)) and the resulting extracts were analyzed by using a PE-Sciex API-3000 HPLC-MS/MS with a heated nebulizer interface (500 degrees C). The method was validated with two different calibration curve ranges, one for etoricoxib (5 to 2500 ng/mL) determined in the presence of lower concentrations of (13)C(6)-etoricoxib (0.5 to 250 ng/mL), and a second curve for the quantitation of similar concentrations of both etoricoxib and (13)C(6)-etoricoxib (0.5 to 250 ng/mL). Extraction recoveries of etoricoxib, (13)C(6)-etoricoxib, and a methylated internal standard were >70% over the range of concentrations included in both calibration curves. Intraday precision and accuracy for the quantitation of etoricoxib were 7.8% relative standard deviation (RSD) or less and within 3.4% respectively over the range of 5 to 2500 ng/mL, and 10.8% RSD or less and within 4 % respectively over the range of 0.5 to 250 ng/mL. Within-batch precision and accuracy for the quantitation of (13)C(6)-etoricoxib over the range of 0.5 to 250 ng/mL were 8.3% RSD or less and within 2.3%, respectively. The validated assay was used in support of human clinical trials.
Asunto(s)
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Colección: 01-internacional Base de datos: MEDLINE Asunto principal: Piridinas / Sulfonas / Isótopos de Carbono / Inhibidores de la Ciclooxigenasa / Isoenzimas Límite: Humans Idioma: En Revista: J Pharm Sci Año: 2002 Tipo del documento: Article País de afiliación: Estados Unidos Pais de publicación: Estados Unidos
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Colección: 01-internacional Base de datos: MEDLINE Asunto principal: Piridinas / Sulfonas / Isótopos de Carbono / Inhibidores de la Ciclooxigenasa / Isoenzimas Límite: Humans Idioma: En Revista: J Pharm Sci Año: 2002 Tipo del documento: Article País de afiliación: Estados Unidos Pais de publicación: Estados Unidos