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A novel rivaroxaban degradant was obtained at 0.45% w/w level during the “RP-HPLC” analysis in the acetic acidexposed rivaroxaban sample. This novel rivaroxaban degradant has a relative retention period (RRT) of approximately 0.95 min. This 0.95 RRT impurity was recognized by LC-MS and then characterized by 1H NMR, 13C NMR, NMR HSQC, NMR HMBC and NMR D2O exchange analyses, and FT-IR techniques. Employed Zorbax XDB C18 eclipse as the main column and Ghost-Guard-LC, ANP00001 as the Ghostbuster column for 0.95 RRT molecule analysis. The mobile phase, phosphate buffer, and acetonitrile mixture, with a simple gradient, were provided to a column at a flow of 1.0 ml/min rate. Samples were evaluated employing a wavelength of 250 nm and injected sample at a volume of 3.0 µL. Good sensitivity was obtained (LOD –0.02% concentration and LOQ – 0.05% concentration) with levels extremely less than allowable limits (0.15%). In the concentration ranges of 0.045% (LOQ) – 0.225% (150% of permissible limits), the technique demonstrated the best linearity for 0.95 RRT molecule analysis, with coefficients of determination of 0.9958. The recovery rate ranged from 93.2% to 105.7%. This approach is shown to be capable of determining 0.95 RRT impurity levels in three rivaroxaban batch samples and one rivaroxaban commercial tablet. |
