Isolation and characterisation of process-related impurities in rofecoxib.


Two unknown impurities in rofecoxib bulk drug at levels below 0.1% were detected by a simple isocratic reverse phase high performance liquid chromatography (HPLC). These impurities were isolated from crude sample of rofecoxib using reverse phase preparative HPLC. (1)H, (13)C and Mass spectroscopic investigations revealed the structures of the impurities as 4-[4-(methylsulphonyl)phenyl]-3-phenyl-5-hydroxyfuran-2-one (I) and 4-[4-(methylsulphonyl)phenyl]-3-phenyl-2,5-furandione (II), respectively. These structures were further confirmed by prepared synthetic standards of the impurities. The tentative mechanism for the formation of these impurities was discussed.

Cite this paper

@article{Reddy2002IsolationAC, title={Isolation and characterisation of process-related impurities in rofecoxib.}, author={K V S R Krishna Reddy and J. Moses Babu and Pramod Kumar Dubey and B V V N Chandra Sekhar and G Om Reddy and Krishnamurthi Vyas}, journal={Journal of pharmaceutical and biomedical analysis}, year={2002}, volume={29 1-2}, pages={355-60} }