顶空气相色谱-电子捕获检测器法测定原料药中痕量的卤代烷烃  

Determination of Trace Haloalkanes in Drugs by Headspace Gas Chromatography with Electron Capture Detector

作　　者：李闫飞 柳文俊 王珏 Li Yanfei;Liu Wenjun;Wang Jue(R&D center of Guangdong Jiabo Pharmaceutical Co.,Ltd.,Qingyuan 511517,China)

机构地区：[1]广东嘉博制药有限公司研发中心,广东清远511517

出　　处：《广东化工》2021年第10期209-210,233,共3页Guangdong Chemical Industry

摘　　要：采用顶空气相色谱-电子捕获检测器法,建立了药料原中基因毒性杂质卤代烷烃(以1-溴丁烷为例)的测定方法,并对方法进行了系统的方法学验证。方法采用以100%二甲基聚硅氧烷(或极性相近)为固定液的毛细管柱为色谱柱进行分离、电子捕获检测器检测、外标法定量的分析方案,实现了药料原中卤代烷烃的检测。1-溴丁烷在线性范围内线性关系良好,线性相关系数(r)为0.9992,定量限为48 ng/mL,定量限6针精密度为7.81%。A method for the determination of genotoxic impurity haloalkanes(1-Bromobutane as an example)in pharmaceutical raw materials was established by headspace gas chromatography with electron capture detector,and the method was systematically verified.Methods a capillary column with 100%dimethylpolysiloxane(or similar polarity)as stationary liquid was used for separation,electron capture detector(ECD)detection and external standard method for quantitative analysis.The linear correlation coefficient(R)was 0.9992.The limit of quantitation(LOQ)was 48 ng/ml and the precision was 7.81%.

关 键 词：基因毒性杂质 卤代烷烃 1-溴丁烷 顶空气相色谱-电子捕获检测器法 外标法 

分 类 号：TQ469[化学工程—制药化工]