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To establish an HPLC-MS/MS method for the determination of the genotoxic impurities (S)-5-chloro-N-(3-chloro-2-hydroxypropyl) thiophene-2-amide and 4-(3-oxy-4-morpholine) nitrobenzene in rivaroxaban. The factors affecting impurities separation and the response of mass spectrometry were systematically investigated.
A ZORBAX SB-C18 column(150 mm×2.1 mm, 3.5 μm) was used with 10 mmol·L-1 ammonium formate solution-methanol as mobile phase at flow rate of 0.4 mL·min-1. And MRM detection by electrospray positive ionization was used.
(S)-5-chloro-N-(3-chloro-2-hydroxypropyl) thiophene-2-amide and 4-(3-oxy-4-morpholine) nitrobenzene had good linear relationships in the range of 0.008-3.4 ng·mL-1 and 0.2-3.4 ng·mL-1, respectively. The average recoveries(n=9) were 97.9% and 98.9%, RSD were 0.94% and 0.68% respectively. The limits of quantitation were 0.008 ng·mL-1 and 0.2 ng·mL-1 respectively. The results of genotoxic impurity residue determination in 15 batches of rivaroxaban samples were far below the limit value.
The method is sensitive and specific, and can effectively detect trace genotoxic impurities in rivaroxaban.
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| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |
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