气相色谱法测定盐酸苯海索中潜在基因毒性杂质  

Determination of Potentially Genotoxic Impurity in Trihexyphenidyl Hydrochloride by GC

作　　者：贝红霞 梁中卫 孔凯丽[1] 丁爱忠[1] Bei Hongxia;Liang Zhongwei;Kong Kaili;Ding Aizhong(Preparation Technology Office Jiangsu Tasly Diyi Pharmaceutical Co.,Ltd.,Huaian 223003,China)

机构地区：[1]江苏天士力帝益药业有限公司制剂技术室,江苏淮安223003

出　　处：《广东化工》2020年第18期160-161,171,共3页Guangdong Chemical Industry

摘　　要：目的建立气相色谱法测定盐酸苯海索中潜在基因毒性杂质氯代环己烷。方法:以DB-624(30 m×0.32 mm,1.8μm)为色谱柱,程序升温;氮气为载气,流速为2.0 mL/min;采用FID检测器,检测器温度为250℃;进样口温度为160℃,进样量为1.0μL,分流比为5∶1。结果:氯代环己烷在1.5167~15.1668μg/mL范围内线性关系良好(r=0.9999),检测限为0.4550μg/mL,定量限为1.5167μg/mL,加标回收率平均值为101.0%(RSD=1.14%,n=9)。结论:该方法准确、简便,适合于盐酸苯海索中潜在基因毒性杂质氯代环己烷的测定。Objective To establish a GC method for the determination of the potentially genotoxic impurity chlorocyclohexane in trihexyphenidyl hydrochloride.Methods A DB-624 column(30 m×0.32 mm,1.8μm)(temperature programming),nitrogen as carrier gas(flow rate:2.0 mL·min-1)and FID(temperature:250℃)were used.Injection port temperature was 110℃,injection volume was 1.0μl and the split ratio was 5:1.Results The calibration curve was well linear for chlorocyclohexane in the range of 1.5167~15.1668μg·mL-1(r=0.9999).The LOD and LOQ were 0.4550μg·mL-1 and 1.5167μg·mL-1,respectively.The average recovery was 101.0%,with RSD of 1.14%(n=9).Conclusion The method is accurate and convenient.It is suitable for the determination of the potentially genotoxic impurity chlorocyclohexane in trihexyphenidyl hydrochloride.

关 键 词：氯代环己烷 潜在基因毒性杂质 盐酸苯海索 气相色谱法 

分 类 号：O65[理学—分析化学]