LC-MS/MS法确认苯扎溴铵中杂质结构及杂质含量测定  

Determination of Impurity Structure and Content in Benzalkonium Bromide by LC-MS/MS Method

作　　者：陈海清 徐雄飞 蔡军民 饶高堂 游谦雄 CHEN Haiqing;XU Xiongfei;CAI Junmin;RAO Gaotang;YOU Qianxiong(Jiangxi Drug Inspection Center,Nanchang Jiangxi 330029,China;Jiangxi Kelun Pharmaceutical Co.,Ltd,Fuzhou Jiangxi 331800,China)

机构地区：[1]江西省药品检查员中心,江西南昌330029 [2]江西科伦药业有限公司,江西抚州331800

出　　处：《药品评价》2024年第10期1191-1194,共4页Drug Evaluation

摘　　要：目的确认苯扎溴铵中杂质化合物并建立测定其含量的方法。方法通过高效液相色谱-质谱法确定杂质为二苄基二甲基溴化铵,用HPLC法测定二苄基二甲基溴化铵的含量,色谱柱为Inertsil ODS-3(4.6 mm×250 mm,5μm),以0.1 mol/L醋酸钠溶液(用冰醋酸调节pH至5.0±0.5)-乙腈(75∶25)为流动相,检测波长为254 nm,流速1.0 mL/min,柱温25℃。结果二苄基二甲基溴化铵在0.5513~77.182μg/mL范围内线性关系良好(r=0.9999),精密度试验RSD为0.53%,平均回收率为100.61%(RSD=1.37%)。结论所建立的检测方法重现性好、操作简便,可用于苯扎溴铵的有关物质控制。Objective To confirm the impurity compounds in benzalkonium bromide and establish a method for its determination.Methods The impurity was determined to be dibenzyl dimethylammonium bromide by high performance liquid chromatography-mass spectrometry.The content of dibenzyl dimethylammonium bromide was determined by HPLC on Inertsil ODS-3 column(4.6 mm×250 mm,5μm).0.1 mol/L sodium acetate solution(pH adjusted to 5.0±0.5 by glacial acetic acid)-acetonitrile(75∶25)was used as the mobile phase.The flow rate of the mobile phase was 1.0 mL/min,the detection wavelength was 254 nm,and the column temperature of the chromatographic column was 25℃.Results Dibenzyl dimethylammonium bromide showed a good linear relationship(r=0.9999)in the range of 0.5513-77.182μg/mL.The average recovery was 100.61%(RSD=1.37%)and the precision RSD was 0.53%.Conclusion The method is simple,reliable and reproducible,can be used to benzalkonium bromide with material control.

关 键 词：苯扎溴铵 二苄基二甲基溴化铵 LC-MS/MS 杂质 含量 

分 类 号：O657.63[理学—分析化学] R927.2[理学—化学]