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To study the related substances in salbutamol sulfate inhalation aerosol during national drug sampling and testing, and to compare the impurity content and evaluate the quality between samples from various enterprises.
HPLC external standard method was utilized to simultaneously determine the content of related substances A, B, C, D, E, F, G, H, I, J, N, and other unknown impurities in salbutamol sulfate inhalation aerosol. Thermo Synchronis C8 chromatography column (250 mm×4.6 mm, 5 μm) was used. Sodium heptane sulfonate solution-acetonitrile was used as the mobile phase. Linear gradient elution was performed and the flow rate was 1.0 mL·min-1. Column temperature was 40 ℃ and detection wavelength was 220 nm. Injection volume was 20 μL. The sources of impurities through forced degradation experiments were explored. Toxicity prediction software for impurity toxicity assessment was applied.
After method validation, the specificity of the method was good, and the separation degree between each impurity peak was greater than 1.5. RSDs of precision test were 0.30%-1.7%(n=6)；mass concentrations of linear range were from 0.050 to 5.000 μg·mL-1(r=0.999 9). Limit of quantitative was in the range of 0.025-0.200 μg·mL-1, limit of detection was in the range of 0.008-0.070 μg·mL-1. The repeatability RSD of raw materials was 0.80%-3.8%, and the recovery rate was 95.2%-104.8%. The repeatability RSD of inhaled aerosol was 1.2%-2.9%, and the recovery rate was 98.7%-102.8%. The forced degradation test showed that impurities D, F, I, J, and N were all degradation impurities. 110 batches of samples were checked and the results of the relevant substances met the regulations. In the samples of diverse enterprises, impurities C, D, F, and N were detected more frequently, while impurities E, G, and H were not detected. Impurity J was only detected in one batch. The predicted impurity D by QSAR software falls to ICH M7 (R2) level 2.
The established method is sensitive and accurate, and can accurately quantify the content of related substances in salbutamol sulfate aerosol, providing effective technical support for systematic supervision. Further toxicity studies should be conducted on impurity D and reasonable limits should be established.
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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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