气相色谱法检测溴芬酸钠中N-亚硝基二甲胺

Determination of N-nitrosodimethylamine in Bromfenac Sodium by Gas Chromatography

采用气相色谱法,建立了溴芬酸钠原料药中基因毒性杂质N-亚硝基二甲胺(NDMA)含量的检测方法。采用Agilent DB-WAX气相色谱柱、氢火焰离子化检测器,液体进样,按外标法测定溴芬酸钠原料药中的NDMA含量。结果表明,NDMA在0.491~24.545μg/mL范围内线性关系良好,定量限(LOQ)为0.48μg/mL,检测限(LOD)为0.24μg/mL;准确度实验回收率为92.4%~104.9%,平均回收率为100.9%,RSD(n=9)为4.4%。该方法操作简单,能够有效地检测溴芬酸钠原料药中NDMA的含量。

The genotoxic impurity N-nitrosodimethylamine(NDMA)in bromfenac sodium was determined by GC analytical method.Agilent DB-WAX was used for GC column,flame ionization detector and direct liquid introduction was used for the detection.An external standard method was established for the determination of NDMA in bromfenac sodium API.The results showed that NDMA had a good linear relationship within the concentration range of 0.491~24.545μg/mL.The limit of quantitation(LOQ)and limit of detection(LOD)of NDMA were 0.48μg/ml and 0.24μg/mL,respectively.The spike recovery of accuracy test was 92.4%~104.9%,average recovery was 100.9%and RSD(n=9)was 4.4%.The method is simple to operated,and it can effectively detect NDMA in bromfenac sodium.