Liquid-Chromatographic Separation and Determination of Process-related Impurities, Including a Regio-Specific Isomer of Celecoxib on Reversed-Phase C18 Column Dynamically Coated with Hexamethyldisilazane
| Autor: | S. Ravikanth, A. Raghuram Rao, D. Nagaraju, S. Meena, R. Nageswara Rao |
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| Rok vydání: | 2006 |
| Předmět: |
Acetonitriles
Chemistry Organic Chemistry Techniques Analytical Analytical Chemistry chemistry.chemical_compound Impurity Phase (matter) Cyclooxygenase Inhibitors Organosilicon Compounds Related impurities Acetonitrile chemistry.chemical_classification Chromatography Sulfonamides Chemistry Temperature Reproducibility of Results Water Hydrogen-Ion Concentration Silanes Sulfonamide Chromatographic separation Models Chemical Celecoxib Silanization Scientific method Pyrazoles Chromatography Liquid |
| Zdroj: | Analytical Sciences. 22:1257-1260 |
| ISSN: | 1348-2246 0910-6340 |
| DOI: | 10.2116/analsci.22.1257 |
| Popis: | A simple and rapid reversed-phase high-performance liquid-chromatographic method for the separation and determination of process-related impurities of celecoxib (CXB) in bulk drugs and pharmaceuticals was developed. The separation of impurities viz., 4-methylacetophenone (I), 1-(4-methylphenyl)-4,4,4-trifluorobutane-1,3-dione (II), 4-hydrazinobenzene sulfonamide (III) and a regio-specific isomer [3-(4-methylphenyl)-5-trifluoromethyl-1H-pyrazole-1-yl]-benzenesulfonamide (IV), was accomplished on an Inertsil ODS-3 column dynamically coated with 0.1% hexamethyldisilazane (HMDS) in acetonitrile:water (55:45 v/v) as a mobile phase and detection at 242 nm using PDA at ambient temperature. The chromatographic conditions were optimized by studying the effects of HMDS, an organic modifier, time of silanization and column temperature. The method was validated and found to be suitable not only for monitoring the synthetic reactions, but also to evaluate the quality of CXB. |
| Databáze: | OpenAIRE |
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