Reference

Development and validation of an HPLC method for the impurity and quantitative analysis of etoricoxib

Development and validation of an HPLC method for the impurity and quantitative analysis of etoricoxib. Hartman, Robert; Abrahim, Ahmed; Clausen, Andrew; Mao, Bing; Crocker, Louis S.; Ge, Zhihong (Analytical Research, Merck Research Laboratories, Rahway, NJ 07065-0914, USA). Journal of Liquid Chromatography & Related Technologies, 26(15), 2551-2566 (English) 2003 Marcel Dekker, Inc. CODEN: JLCTFC. ISSN: 1082-6076. DOCUMENT TYPE: Journal CA Section: 64 (Pharmaceutical Analysis) Etoricoxib (5-chloro-6'-methyl-3[4-(methanesulfonyl)phenyl]-2,3'-bipyridine) is a highly active and selective cyclo-oxygenase II inhibitor.Some commonly used reagents like 646459-40-7 and 202409-33-4 are used in this experiment. A single, stability-indicating HPLC method was developed and validated for both the impurity and quant. anal. of etoricoxib. Method development incorporated the optimization of stationary phase, pH, temp., and mobile phase compn. for the resoln. of 13 process impurities and 3 major degrdn. products. Further optimization of pH and mobile phase compn. was aided by the use of DryLab, a computer-based simulation program. The stability-indicating capability of the method was proven through the identification of photolytic and oxidative decompn. products. Method validation produced excellent results for linearity, precision, limit of quantitation and limit of detection, specificity, accuracy, recovery, and robustness. The identities of etoricoxib decompn. products were confirmed by UV, LC/MS, and NMR spectra. .

Validated liquid chromatographic ultraviolet method for the quantitation of Etoricoxib in human plasma using liquid-liquid extraction

Validated liquid chromatographic ultraviolet method for the quantitation of Etoricoxib in human plasma using liquid-liquid extraction. Ramakrishna, N. V. S.; Vishwottam, K. N.; Wishu, S. 202409-33-4 are also occured in this study.; Koteshwara, M. ( Biopharmaceutical Research, Suven Life Sciences Ltd., Hyderabad 500034, India). Journal of Chromatography, B: Analytical Technologies in the Biomedical and Life Sciences, 816(1-2), 215-221 (English) 2005 Elsevier B.V. CODEN: JCBAAI. ISSN: 1570-0232. DOCUMENT TYPE: Journal CA Section: 1 (Pharmacology) A simple, sensitive and specific HPLC method with UV detection (284 nm) was developed and validated for quantitation of Etoricoxib in human blood plasma, the newest addn. to the group of nonsteroidal anti-inflammatory drugs - a highly selective cyclooxygenase-2 inhibitor. Following a single-step liq.-liq. extn. with di-Et ether/dichloromethane (70/30, vol./vol.), the analyte and internal std. (Zaleplon) were sepd. using an isocratic mobile phase of water/acetonitrile (58/42, vol./vol.) on reverse phase Waters symmetry C18 column. The lower limit of quantitation was 5 ng/mL, with a relative std. deviation of < 20%. A linear range of 5-2500 ng/mL was established. This HPLC method was validated with between- and within-batch precision of 4.1-5.1% and 1.1-2.4%, resp. The between- and within-batch bias was -3.8-4.7% and -0.6-9.4%, resp. Frequently coadministered drugs did not interfere with the described methodol. Stability of Etoricoxib in plasma was >90%, with no evidence of degrdn. during sample processing (autosampler) and 30 days storage in a freezer. This validated method is sensitive and simple with between-batch precision of <6% and was used in pharmacokinetic studies. .