LC-MS法测定氨磷汀原料药中的N-(2-溴乙基)-1,3-丙二胺二氢溴酸盐  

Determination of N-(2-bromoethyl)-1,3-propane-diamine dihydrobromide in Amifostine by LC-MS

作　　者：王倩 王雪芹[1] 朱艳春 吕海鸿[1] 张竞[1] WANG Qian;WANG Xueqin;ZHU Yanchun;LU Haihong;ZHANG Jing(Henan Provincial Institute for Food and Drug Control,Zhengzhou,Henan,450008 P.R.China)

机构地区：[1]河南省食品药品检验所,河南郑州450008

出　　处：《华西药学杂志》2023年第4期441-443,共3页West China Journal of Pharmaceutical Sciences

基　　金：河南省市场监督管理局科技计划项目(2020sj27)。

摘　　要：目的采用LC-MS法测定氨磷汀原料药中N-(2-溴乙基)-1,3-丙二胺二氢溴酸盐的含量。方法样品用水溶解稀释,采用Waters CORTECSⓇT3色谱柱(100 mm×2.1 mm,2.7μm),流动相为0.1%七氟丁酸水溶液-0.1%七氟丁酸乙腈,梯度洗脱,柱温35℃,流速0.3 mL·min-1,进样量5μL。质谱采用电喷雾正离子模式,多反应监测,检测离子对为m/z 181.0→136.0、m/z181.0→106.7。按外标法进行定量。结果N-(2-溴乙基)-1,3-丙二胺二氢溴酸盐的线性范围为10.17~203.31 ng·mL^(-1)(r=0.9985),检出限为5.08 ng·mL^(-1),定量限为10.17 ng·mL^(-1);仪器的精密度和方法重复性的RSD均<10%;平均回收率为85.8%,RSD=2.9%(n=6);3批样品中均未检出N-(2-溴乙基)-1,3-丙二胺二氢溴酸盐。结论所用方法简单、高效、重复性好,可用于检测氨磷汀原料药中N-(2-溴乙基)-1,3-丙二胺二氢溴酸盐的含量。OBJECTIVE To determine N-(2-bromoethyl)-1,3-propane-diamine dihydrobromide in Amifostine by LC-MS.METHODS Sample was dissolved and diluted with water.The determination was performed on Waters CORTECSⓇT3 column(100 mm×2.1 mm,2.7μm)with 0.1%heptafluorobutyric acid-water solution and 0.1%heptafluorobutyric acid-acetonitrile as the mobile phase with elution gradient.The flow rate was 0.3 mL·min-1,the column temperature was 35℃,and the sample volume was 5μL.The analytes were analyzed by electro-spray ionization(ESI)in the multiple reaction monitoring mode with positive ion.The precursors of production transitions of m/z impurity181.0→136.0 and 181.0→106.7,were used to measure impurity,quantitated by the external reference method.RESULTS The N-(2-bromoethyl)-1,3-propane-diamine dihydrobromide showed a good linear relationship(r=0.9985)in the concentration range of 10.17-203.31 ng·mL^(-1).The LODs was 5.08 ng·mL^(-1),and the LOQs was 10.17 ng·mL^(-1).The RSDs of precision and repeatability were less than 10%.The average recovery was 85.8%,with the RSD of 2.9%(n=6).The content of N-(2-bromoethyl)-1,3-propane-diamine dihydrobromide were less than the LOD in the three batches of samples tested.CONCLUSION This method is simple,efficient and repeatable,which can be used to determine the content of N-(2-bromoethyl)-1,3-propane-diamine dihydrobromide in Amifostine.

关 键 词：液质联用色谱法 氨磷汀 N-(2-溴乙基)-1 3-丙二胺二氢溴酸盐 外标法 含量测定 多反应监测 遗传毒性杂质 

分 类 号：R917[医药卫生—药物分析学]