摘要
目的建立食品和生物体等中毒样本中毒鼠强、氟乙酰胺、氟乙酸钠3种致痉挛性杀鼠剂的气相色谱质谱联用仪(GC-MS)快速确认方法。方法样品经液-液萃取、氮吹浓缩后毒鼠强、氟乙酰胺直接上GC-MS进行定性确认与定量检测,氟乙酸钠需要进一步微波衍生后上GC-MS测试。结果该方法氟乙酰胺与毒鼠强的定量下限均为0.2 mg/kg,氟乙酸钠定量下限为1.0 mg/kg,3种杀鼠剂的相对标准偏差(RSD)在2.27%~8.54%之间,回收率在63.3%~92.62%之间,线性相关系数r均大于0.999。结论该方法简单、快速、准确可靠,适用于食品和生物体等中毒检材中毒鼠强、氟乙酰胺、氟乙酸钠3种致痉挛性杀鼠剂的快速气象色谱质谱确证。
[Objective]To establish a method for rapid determination of 3 kinds of spasms-causing raticide(tetramine,fluoroacetamide and sodium fluroacetate)in poisoning samples such as food and biological fluids by gas chromatography-mass spectrometry(GC-MS).[Methods]The samples were extracted by liquid-liquid extraction and concentrated by nitrogen. The qualitative confirmation and quantitative detection of tetramine and fluoroacetamide were performed by GC-MS directly. The sodium fluroacetate were determined by GC-MS after microwave assisted derivatization.[Results]The lower limit of quantitation for tetramine and fluoroacetamide were both 0.2 mg/kg,and that for sodium fluroacetate was 1.0 mg/kg. The relative standard deviation(RSD) of 3 kinds of raticide was 2.27%-8.54%,the recoveries were between 63.3% and 92.62%,and the correlation coefficients(r)for the linear equation were above 0.999.[Conclusion] The method is simple,rapid,accurate and sensitive,which is suitable for the quick confirmation of spasms-causing raticide(tetramine,fluoroacetamide and sodium fluroacetate) in poisoning samples such as food and biological fluids by GC-MS.
出处
《职业与健康》
CAS
2017年第14期1906-1909,共4页
Occupation and Health
基金
深圳市卫生计生系统科研项目(201303222)
关键词
气相色谱质谱联用仪
致痉挛性杀鼠剂
氟乙酰胺
微波衍生
Gas chromatography-mass spectrometry
Spasms-causing raticide
Fluoracetamide
Microwave assisted derivatization