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中国药物评价 ›› 2024, Vol. 41 ›› Issue (1): 61-64.

• 评价技术与方法 • 上一篇    下一篇

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

岳青阳, 陈默, 徐万魁*   

  1. 辽宁省检验检测认证中心,辽宁省药品检验检测院/国家药品监督管理局化学
         药品质量研究与评价重点实验室, 辽宁 沈阳 110036
  • 收稿日期:2023-06-30 修回日期:2023-10-18 出版日期:2024-02-28 发布日期:2024-02-28

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

  1. Liaoning Inspection, Examination and Certification Centre, Liaoning Institute for Drug Control/NMPA Key Laboratory
         for Quality Research and Evaluation of Chemical Drug, Liaoning Shenyang 110036, China
  • Received:2023-06-30 Revised:2023-10-18 Online:2024-02-28 Published:2024-02-28

摘要: 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。

关键词: 气相色谱仪-质谱联用仪(GC-MS), 环氧氯丙烷, 3-氯丙烯

Abstract: 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=0.999 8). The detection limit and the quantification limit were 0.522 0 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.

Key words: Gaschromatography-mass spectrometry(GC-MS), Epichlorhydrin, 3-chloropropene

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