摘要
目的建立衍生化GC-MS法测定左氧氟沙星中潜在基因毒性杂质二氯亚砜。方法采用DB-624毛细管柱(30m×0.32mm×1.8μm),程序升温;离子源温度230℃,四极杆温度150℃,SIM模式m/z79.00;进样口温度为210℃;顶空平衡温度为90℃,平衡时间为30min;以甲醇为溶剂衍生化二氯亚砜。结果二氯亚砜质量浓度在19.98~199.80ng·mL^-1范围内线性关系良好(r2=0.9927);检测限为9.99ng·mL^-1,定量限为19.98ng·mL^-1;平均回收率为88.6%(RSD=5.5%,n=9);重复性良好(RSD=4.4%,n=6)。3批原料药中未检出二氯亚砜。结论经方法学验证,本法适用于左氧氟沙星中二氯亚砜的测定。
OBJECTIVE To develop a GC-MS method for the determination of the dichlorosulfane potentially genotoxic impurity in levofloxacin.METHODS A DB-624(30m×0.32mm×1.8μm)column was adopted with a gradient elutionsystem.RESULTS The calibration curve was linear for dichlorosulfane in the range of 19.98-199.80ng·mL^-1(r 2=0.9927).The limit of detection and limit of quantification were 9.99ng·mL^-1 and 19.98ng·mL^-1,respectively.The average recovery was 88.6%,with RSD of 5.5%(n=9).The repeatability was fine,withRSD of 4.4%(n=6).The impurity was not detected in three batches of levofloxacin.CONCLUSION The method was applicable for the quality control of dichlorosulfane in levofloxacin through the methodology validation.
作者
陈爽
黄巧巧
CHEN Shuang;HUANG Qiao-qiao(Zhejiang Institute of Food and Drug Control,Hangzhou 310052,China)
出处
《海峡药学》
2019年第5期54-56,共3页
Strait Pharmaceutical Journal