首页|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

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

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

Gaschromatography-mass spectrometry(GC-MS)Epichlorhydrin3-chloropropene

岳青阳、陈默、徐万魁

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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

气相色谱仪-质谱联用仪(GC-MS) 环氧氯丙烷 3-氯丙烯

2024

中国药物评价
国家食品药品监督管理局信息中心

中国药物评价

影响因子:1.09
ISSN:2095-3593
年,卷(期):2024.41(1)
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