衍生化-气相色谱法测定枸橼酸托瑞米芬中遗传毒性杂质  

Determination of Genotoxic Impurities in Toremifene Citrate by Derivatization GC

作　　者：陈端腾 杨书宇 陈锋 CHEN Duanteng;YANG Shuyu;CHEN Feng(Nanjing H&D Pharmaceutical Technology Co.,Ltd.,Jiangsu Nanjing 210046;School of Chemistry and Chemical Engineering,Yangzhou University,Jiangsu Yangzhou 225009,China)

机构地区：[1]南京恒道医药科技股份有限公司,江苏南京210046 [2]扬州大学化学化工学院,江苏扬州225009

出　　处：《广州化工》2025年第6期113-116,共4页GuangZhou Chemical Industry

摘　　要：建立衍生化测定枸橼酸托瑞米芬中2-氯乙胺和2-氯-N-甲基乙胺含量的气相色谱法。采用以(5%-苯基)-甲基聚硅氧烷为固定液的(Agilent HP-5)毛细管色谱柱分离,氢火焰离子化检测器检测。2-氯乙胺在1.652~99.11μg·mL^(-1)范围内线性关系良好,r=0.9999,检出限0.6608μg·mL^(-1)。2-氯-N-甲基乙胺在0.660~99.04μg·mL^(-1)范围内线性关系良好,r=0.9999,检出限0.3301μg·mL^(-1)。2-氯乙胺的平均回收率为107.2%,RSD为3.6%(n=9)。2-氯-N-甲基乙胺的平均回收率为111.9%,RSD为2.2%(n=9)。该方法为研究其他药物中此类遗传毒性杂质的检测提供了一种可靠的参考。To establish a derivatization GC method for the determination of 2-Chloroethanamine and 2-Chloro-NMethylethanamine in Torremiphene citrate API,Agilent HP-5 capillary column and FID were used for separating and detecting the analytes.2-chloroethanamine showed good linearity at the concentration range of 1.652~99.11μg·mL^(-1)(r=0.9999).The LOD was 0.6608μg·mL^(-1).The average recovery was 107.2%,and RSD was 3.6%(n=9).2-chloro-Nmethylethanamine showed good linearity at the concentration range of 0.6602 to 99.04μg·mL^(-1).LOD was 0.3301μg·mL^(-1).The average recovery was 111.9%,and RSD was 2.2%(n=9).The method provided a reference for the detection of similar impurities in other drugs.

关 键 词：气相色谱 遗传毒性杂质 枸橼酸托瑞米芬 2-氯乙胺 2-氯-N-甲基乙胺 

分 类 号：R917[医药卫生—药物分析学]