GC法测定潜在基因毒性杂质1-(1-氯乙基)-2,3-二甲基苯  

Determination of Potential Genotoxic Impurity 1- (1-Chloroethyl)-2,3-Dimethylbenzene by GC

作　　者：闵婕 王恩 林萍 兰公剑 MIN Jie;WANG En;LIN Ping;LAN Gong-jian(Nanjing Chia Tai Tianqing Pharmaceutical Co.,Ltd.,Nanjing Jiangsu 210046,China)

机构地区：[1]南京正大天晴制药有限公司,江苏南京210046

出　　处：《辽宁化工》2022年第3期442-444,共3页Liaoning Chemical Industry

摘　　要：建立了潜在基因毒性杂质1-(1-氯乙基)-2,3-二甲基苯的GC-FID检测方法。采用DB-624(30 m×0.32 mm,1.8µm)毛细管色谱柱,柱温为程序升温,载气流速为2.0 mL·min^(-1),进样口温度为280℃,检测器温度为280℃,进样量为1.0μL,分流比为10∶1。结果表明:1-(1-氯乙基)-2,3-二甲基苯在0.92~13.82μg·mL^(-1)范围内线性关系良好(r=0.9998),检测限为0.46μg·mL^(-1),定量限为0.92μg·mL^(-1),加标回收率平均值为115.7%(RSD=1.5%,n=9)。该方法灵敏度高,准确简便,适用于潜在基因毒性杂质1-(1-氯乙基)-2,3-二甲基苯的测定。A method for the determination of the potentially genotoxic impurity 1-(1-chloroethyl)-2,3-dimethylbenzene by GC-FID was established.A DB-624 was used as capillary column(30 m×0.32 mm,1.8μm)(temperature programming),carrier gas flow rate was 2.0 mL·min^(-1),injection temperature and FID temperature both were 280℃.Injection volume was 1.0μL and the split ratio was 10∶1.The calibration curve was well linear for 1-(1-chloroethyl)-2,3-dimethylbenzene in the range of 0.92~13.82μg·mL^(-1)(r=0.9998).The LOD and LOQ were 0.46μg·mL^(-1) and 0.92μg·mL^(-1),respectively.The average recovery was 115.7%,with RSD of 1.5%(n=9).The method is sensitive,accurate and convenient.It is suitable for the determination of the potential genotoxic impurity 1-(1-chloroethyl)-2,3-dimethylbenzene.

关 键 词：1-(1-氯乙基)-2 3-二甲基苯 潜在基因毒性杂质 气相色谱法 

分 类 号：O657.7[理学—分析化学]