GC-MS法测定阿替洛尔原料中基因毒性杂质环氧氯丙烷

Determination of the Genotoxic Impurity Epichlorohydrin in Atenolol by GC-MS

目的:建立气相质谱分析方法测定阿替洛尔原料中的基因毒性杂质环氧氯丙烷。方法:采用DB-624 UI(30 m×0.32 mm×1.8μm)毛细管柱,起始温度60℃,载气流速为1.5 mL·min^(-1),进样口温度为220℃。质谱方法采用选择离子监测(SIM)模式,m/z为49和62。结果:环氧氯丙烷在0.0354~0.7088μg·mL^(-1)范围内线性良好(r=1.0000),加样回收率为98%,RSD=1%(n=9),最低检测限为0.0177μg·mL^(-1)。结论:本方法灵敏度高,专属性好,可用于阿替洛尔原料中环氧氯丙烷的监测。

Objective:To establish a gas chromatography-mass spectrometry(GC-MS)method for the determination of epichlorohydrin in atenolol.Method:The samples were separated on an DB-624 UI(30 m×0.32 mm×1.8μm)capillary column.The column temperature was maintained at 60℃,and then gradiently raised to 220℃.The flow rate of carrier gas was 1.5 mL·min^(-1).Selected ion monitoring(SIM)was adopted for mass spectrometry,and m/z was 49 and 62.Results:The assay linearity of epichlorohydrin was confirmed over the range of 0.0354~0.7088μg·mL^(-1)(r=0.9999).The average recovery of epichlorohydrin was 98%and the RSD was 1%(n=9).The limit of determination was 0.0177μg·mL^(-1).Conclusion:The method is sensitive and specific,which is suitable for the determination of epichlorohydrin in atenolol.