Srinivasu M K, Narayana C L, Rao D S, Reddy G O
Analytical Research, Dr Reddy's Research Foundation, Miyapur, Hyderahad, India.
J Pharm Biomed Anal. 2000 Jul;22(6):949-56. doi: 10.1016/s0731-7085(00)00303-4.
A new reversed-phase, isocratic LC method was developed for the quantitative determination of COX-2 inhibitor celecoxib in bulk drugs and in pharmaceutical dosages. The proposed method is also applicable for the purity evaluation of celecoxib in bulk drugs. 5-Methyl 2-Nitro phenol has been used as internal standard for the quantitative determination of celecoxib. The method has been completely validated and proven to be rugged. The limit of detection (LOD) and limit of quantitation (LOQ) for celecoxib impurities namely, 4-hydrazino benzene sulfonamide (Intermediate I) and 1-(4-methyl phenyl)-4,4.4-trifluro butan-1,3-dione (Intermediate II) were found to be 32.0 and 97 ng. respectively. The active pharmaceutical ingredient was extracted from its finished dosage form (capsule) using methanol. The percentage recoveries ranged from 90.7 to 93.8. The stability studies were performed for celecoxib solution placed on laboratory bench and in refrigerator for hundred days. The samples were found to be stable for the study period.
