关键词: font-size:medium, ">GC法；基因毒性杂质；二甲基苯胺；二甲基硝基苯

Abstract: Objective：To establish GC method for simultaneous determination of seven potential genotoxic impurities in amide API intermediate. Methods：The chromatographic separation was performed on a capillary column of HP-INNOWAX（60 m× 0.32 mm× 0.25 μm）， the initial temperature was 80 ℃， and the temperature was raised to 130 ℃ at a rate of 20 ℃ per minute for 30 min， and then to 250 ℃ at a rate of 12 ℃ per minute for 15 min， the inlet temperature and the FID detector temperature were set at 200 ℃ and 260 ℃， the flow rate was 1.5 mL·min-1， and the split ratio was 2∶1.Results：The linear ranges of 2，6-dimethylnitrobenzene，2，5-dimethylnitrobenzene，2，4-dimethylaniline，2，5-dimethylaniline，2，4-dimethylnitrobenzene，2，3-dimethylnitrobenzene and 2，3-dimethylaniline were 0.391 8-156.7 μg·mL-1（r=0.998），0.391 5-7.830 μg·mL-1（r=0.999），0.787 6-15.75 μg·mL-1（r=0.999），0.398 8-15.95 μg·mL-1（r=0.999），0.211 9-8.475 μg·mL-1（r=0.999），0.196 8-7.871 μg·mL-1（r=0.999），0.204 2-16.34 μg·mL-1（r=0.999）， respectively. They have good linear relationship with peak area. The average recoveries（n=9） were 89.58%、88.18%、89.50%、88.99%、86.88%、89.53%、88.32%，respectively， with RSDs less than 10%.Conclusion：The established GC method can simultaneously determine seven potential genotoxic impurities， which provides a new method for the quality control of amide API intermediate.

Key words: font-size:medium, ">GC method； Genotoxic impurity； Dimethylaniline； Dimethylnitrobenzene