GC-MS法测定氯沙坦钾中痕量的N-亚硝基二甲胺和N-亚硝基二乙胺

Determination of trace N-nitrosodimethylamine and N-nitrosodiethylamine in Losartan potassium by GC-MS

目的测定氯沙坦钾中痕量的基因毒性杂质N-亚硝基二甲胺(NDMA)和N-亚硝基二乙胺(NDEA)。方法采用HP-INNOWAX毛细管柱(30 m×0.32 mm,0.5μm),程序升温,电子轰击(EI)离子源和选择离子监测(SIM)模式检测。结果5~125 ng·mL^(-1) NDMA和NDEA的线性关系良好,检测限浓度均为1.7 ng·mL^(-1),相当于样品浓度17 ng·g^(-1),加样回收率为95.1%~104.2%。结论所用方法准确、灵敏、可靠,可用于氯沙坦钾原料药中基因毒性杂质NDMA和NDEA含量的测定。

OBJECTIVE To determine trace genotoxic impurities of N-nitrosodimethylamine(NDMA)and N-nitrosodiethylamine(NDEA)in Losartan potassium.METHODS Samples were separated using HP-INNOWAX capillary column under temperature program,ionized by electron ionization(EI),and detected with selected ion monitoring(SIM)mode.RESULTS NDMA and NDEA were well correlated with the linearity range between 5 ng·mL^(-1) and 125 ng·mL^(-1).Limit of detections both were 1.7 ng·mL^(-1) for NDMA and NDEA,and equivalent to the sample concentration of 17 ng·g^(-1).The average recoveries were between 95.1%and 104.2%.CONCLUSION The method is accurate,sensitive and reliable,which can be used for the determination of NDMA and NDEA in Losartan potassium.