GC-MS法测定头孢泊肟酯中的氯甲烷和氯乙烷  

Determination of chloromethane and chloroethane in cefpodoxime proxetil by a gas chromatography-mass spectrometry method

作　　者：白青山 田朋鑫 BAI Qingshan;TIAN Pengxin(Linyi Inspection and Testing Center,Linyi 276000,China)

机构地区：[1]临沂市检验检测中心,山东临沂276000

出　　处：《药学研究》2021年第6期377-379,408,共4页Journal of Pharmaceutical Research

摘　　要：目的建立一种气相色谱-质谱联用法(GC-MS)对头孢泊肟酯原料药中的基因毒性杂质氯甲烷和氯乙烷进行定量检测。方法采用MEGA-624MS色谱柱(60 m×0.25 mm,1.4μm),以电子轰击电离源为离子源,采集模式为选择离子监测(SIM)。结果氯甲烷在0.2525~1.263μg·mL^(-1)内线性关系良好(r=0.9991),定量限为0.04040 ng·mL^(-1),检出限为0.01616 ng·mL^(-1);氯乙烷在0.6451~3.226μg·mL^(-1)内线性关系良好(r=0.9997),定量限为0.1032 ng·mL^(-1),检出限为0.04129 ng·mL^(-1)。氯甲烷和氯乙烷的回收率分别为100.8%、100.6%。结论经方法学验证,该法可用于同时测定头孢泊肟酯中的氯甲烷和氯乙烷,能为质量控制提供参考。Objective To determine chloromethane and chloroethane,known as potential carcinogenic and genotoxic impurities in cefpodoxime proxetil by gas chromatography-mass spectrometry(GS-MS).Methods The separation was carried out on a MEGA-624MS column,while electron bombardment ionization source(EI)and selective ion monitoring(SIM)mode was used for detection.Results The results showed that chloromethane and chloroethane had a good linear relationship within the concentration range of 0.2525~1.263μg·mL^(-1) and 0.6451~3.226μg·mL^(-1) respectively.The limits of quantitation(LOQ)of chloromethane and chloroethane were 0.04040 ng·mL^(-1) and 0.1032 ng·mL^(-1),and the limits of detection(LOD)were 0.01616 ng·mL^(-1) and 0.04129 ng·mL^(-1),respectively.Recoveries of chloromethane and chloroethane were 100.8%and 100.6%,respectively.Conclusion The methodology validation showed that this GC-MS method could be used as a quality control method for the simultaneous determination of chloromethane and chloroethane in cefpodoxime proxetil.

关 键 词：头孢泊肟酯 氯甲烷 氯乙烷 基因毒性杂质 气相色谱-质谱联用法 

分 类 号：R927.2[医药卫生—药学]