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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
Author(s) -
Nageswara Rao R.,
Meena S.,
Nagaraju D.,
Raghu Ram Rao A.
Publication year - 2005
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.458
Subject(s) - chemistry , chromatography , chromatographic separation , phase (matter) , biological fluids , high performance liquid chromatography , organic chemistry
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 quantication. The linearity range was found to be 1.0–20 µg/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 µg/mL simultaneously. Copyright © 2004 John Wiley & Sons, Ltd.