Full
Outline
To establish a liquid chromatography-tandem mass spectrometry method (LC-MS/MS method) for determination the contents of 5-methyl isoquinoline sulfonic acid (impurity A) and 5-ethyl isoquinoline sulfonic acid (impurity C) which are genotoxic impurities in fashudil hydrochloride.
The LC-MS/MS method was achieved by a Waters Symmetry C18(100 mm×3 mm, 3.5 μm) column utilizing a mobile phase of 0.1% formic acid aqueous solution-acetonitrile with gradient elution at a flow rate of 0.5 mL·min-1. The column temperature was set at 30 ℃, the injection volume was 10 μL. The electrospray was operated with the source ESI under positive ionization scanning mode, and data were collected and analyzed.
Standard curves of impurity A and impurity C have a good linear relationship in the linear range. The limits of detection were 0.2 and 0.02 ng·mL-1, respectively, and the average recovery range was 93.0%~98.0%, RSD<4.67%(n=9). The RSDs of precision, accuracy, stability and durability tests were all less than 10.0%. Impurities A and C in the 3 batches of fashudil hydrochloride were not detected.
The established method was fast, accurate and reproducible, which could be used for the control of genotoxic impurities A and C in fashudil hydrochloride.
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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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