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Objective: To eatablish a UPLC-MS/MS method for determination of three azide-type genotoxics, 5-(4′-(azidomethyl)-[1,1′-biphenyl]-2-yl)-1H-tetrazole (MB-X), 4′-(azidomethyl)-[1,1′-bihenyl]-2-carbonitrile (AZBC), and 5-(4′-((5-azido-2-butyl-4-chloro-1H-imidazol-1-yl)methyl)-[1,1′-biphenyl]-2-yl)-1H-tetrazole (LADX), in active pharmaceutical ingredients (API) of irbesartan and losartan potassium.Methods:The separation was performed on a ACQUITY UPLC HSS T3 column(100 mm×2.1 mm, 1.8 μm) with the mobile phases consisting of 0.1% formic acid aqueous solution (mobile phase A) and 0.1% formic acid methanol solution (mobile phase B) using a gradient elution at a flow rate of 0.35 mL·min-1. The column temperature was set at 50 ℃. Multiplereaction monitoring (MRM) was performed on a triple quadripole mass spectrometer equipped with a APCI source in positive/negative mode.Results:the calibration curve was linear for three compounds in the range of 0.5~100 ng·mL-1. The recoveries (n=3) in irbesartan of low, middle, high concentration-spiked samples are 94.5%~103.5% with RSD<3.88%. The recoveries (n=3) in losartan potassium of low, middle, high concentration-spiked samples are 93.8%~100.9% with RSD<4.25%. The limits of detection are 0.05, 0.03, 0.02 ng·mL-1 and the limits of quantification are 0.15, 0.11, 0.08 ng·mL-1, respectively.Conclusion:The method is sensitive and accurate, which is applicable for quantification of three azide-type genotoxic impurities in irbesartan API and losartan potassium API. The method can provide reference for quality control of irbesartan and losartan potassium.
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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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