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OBJECTIVE To establish a quantitative nuclear magnetic resonance coupled with high performance liquid chromatography (qNMR-HPLC) technique for the rapid determination of cilostazol impurity Ⅰ correction factor. METHODS The mixture of cilostazol and cilostazol impurity Ⅰ was dissolved in deuterated dimethyl sulfoxide. A portion of the solution was determined by qNMR, while the other portion of the solution was diluted with water-acetonitrile (60:40) and analyzed by HPLC. The correction factor of cilostazol impurity Ⅰ was calculated with the response signals from qNMR and the peak areas from HPLC. The correction factor of cilostazol impurity Ⅰ was also determined by HPLC standard curve method. A mixed solution containing residual solvent was prepared to simulate the effect of solvents in determining correction factors. When the content of cilostazol impurity Ⅰ was inaccurately assigned due to residual solvent, difference between qNMR-HPLC method and standard curve method was compared. RESULTS When the contents of cilostazol and cilostazol impurity Ⅰ were assigned accurately, the correction factors for cilostazol impurity Ⅰ by qNMR-HPLC method and HPLC standard curve method were 1.74 and 1.76, respectively, which were basically consistent with the pharmacopoeial results. When cilostazol impurity Ⅰ contained residual solvents, and there was an error in the content assignment, the correction factor of the determination by the qNMR-HPLC technique was still 1.72, and the result was not affected by the accuracy of the content. While the correction factor of HPLC standard curve was 2.01, which was deviated from the actual results. CONCLUSION Compared with the HPLC standard curve method, the qNMR-HPLC coupling technique is independent of the accuracy of the content of the substance to be measured and the weighing volume, and does not require purification to prepare a high purity compound. qNMR-HPLC is a powerful tool in the determination of impurity correction factors.
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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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