GC-MS法结合顶空进样测定环氧氯丙烷中遗传毒性杂质3-氯丙烯的含量

Determination of the Genotoxic Impurity 3-Chloropropene in Epichlorhydrin by GC-MS combined with Headspace Injection

目的:建立环氧氯丙烷中遗传毒性杂质3-氯丙烯的检测方法。方法:色谱柱为Agilent DB-624UI,载气为氦气,流速为1.23 mL·min^(-1),进样口温度250℃,柱温为程序升温。顶空瓶平衡温度为100℃,平衡时间30 min。电子轰击电离方式,离子源温度:230℃;定量测定采用SIM模式。结果:3-氯丙烯在1.044~52.20 ng·mL^(-1)(r=0.999 8)浓度范围内呈良好线性关系,检测限和定量限分别为0.522 0和1.044 ng·mL^(-1),加样回收率为94.13%。结论:该法分离效果好、操作简便、灵敏度高,可监控环氧氯丙烷产品质量。

Objective:To establish a specific method of the genetic toxicity impurity 3-chloropropene in epichlorhydrin.Methods:The chromatographic column was Agilent DB-624UI,the carrier gas was helium,the flow rate was 1.23 mL·min^(-1),the inlet temperature was 250℃,and the column temperature was programmed to increase.The Vials was incubated at 100℃for 30 min.The electron impact ionization method was used,and the ion source temperature was 230℃.The quantitative determination was carried out using the SIM mode.Results:3-chloropropene showed a good linear relationship within the concentration range of 1.044-52.20 ng·mL^(-1)(r=0.9998).The detection limit and the quantification limit were 0.5220 and 1.044 ng·mL^(-1),respectively,and the sample recoveries was 94.13%.Conclusion:The method is good in separation effect,convenient and highly sensitive.It can be used to monitor the quality of epichlorhydrin products.