左氧氟沙星中潜在基因毒性杂质二氯亚砜的GC-MS法测定

Determination of Dichlorosulfane Potentially Genotoxic Impurity in Levofloxacin by GC-MS

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.