Full
Outline
To establish an LC-MS method for the determination of two phenylhydrazine-like genotoxic impurities [(4-sulfamoylphenyl) hydrazine, SHH; (4-methyl-acetophenone) para-sulfonamide phenylhydrazine, MAP] in celecoxib.
The separation was established on Thermo BDS Hypersil C18(100 mm×4.6 mm, 2.4 μm) column by liner gradient elution using (0.1% ammonium formate-0.1% formic acid buffer solution)-methanol 90∶10 as mobile phase A and methanol as mobile phase B. 5 mmol·L-1 dithiothreitol buffer solution was used as the antioxidant, the determination was carried out by multiple reactions monitoring mode with positive electrospray ionization, meanwhile, the analytes were quantitatively determined by internal reference method.
The established LC-MS method displayed satisfactory linearity over the concentration range of 20~200 ng·mL-1. The average recovery was 99.7% (RSD=6.0%) for SHH and 97.6% (RSD=5.1%) for MAP. The limit of detection and limit of quantification were 10 ng·mL-1 and 20 ng·mL-1, respectively. The reference and test solutions were stable at 4 ℃ for 4 h.
The established LC-MS method is suitable for simultaneous determination of SHH and MAP genotoxic impurities in celecoxib.
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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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