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OBJECTIVE To develop a supercritical fluid chromatography method for separation of brivaracetam and its three stereoisomers. METHODS Brivaracetam and its three isomers were separated on a silica gel column coated with amylose-tris (3,5-dimethyl phenylcarbamate) (CHIRALPAK AD, 4.6 mm×250 mm, 10 μm) and maitained at 40 ℃. The mobile phase consisted of a mixture of CO2 and methanol (90∶10). The flow rate was at 2.0 mL min-1 , and the detection wavelength was set at 205 nm. The back pressure of SF-CO2 was set at 18 MPa, and the injection volume was 6 μL. RESULTS Brivaracetam and its three isomers were separated successfully in 10 min with a resolution factor of 2.8, 2.8 and 4.0, respectively. Brivaracetam exhibited a good linear relationship with peak area within the concentration range of 0.01-0.5 mg·mL-1(r=0.999 8, n=8). Isomer A, B, and C also exhibited a good linear relationship with peak area within the concentration range of 0.005-0.5 mg·mL-1 (r=0.999 9, n=9). The detection limits of brivaracetam and its three isomers(S/N=3) were all 2 μg·mL-1, and the quantitation limits(S/N=10) were all 5 μg·mL-1. The average spiked recoveries of three isomers at three different concentration levels were 102.1%, 105.8% and 102.6%, respectively(n=9). CONCLUSION Compared with conventional liquid chromatography, supercritical fluid chromatography can significantly improve the separation efficiency, shorten the separation time, and greatly reduce the amount of alkane organic solvents, which can be effectively used for the quality control of the isomer impurities in brivaracetam tablets.
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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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