兰红军,吴雪梅,冯耀基,黎少映.QuEChERS-气相色谱-串联质谱法测定鸡蛋中氟虫腈及其代谢产物[J].中国食品卫生杂志,2019,31(5):435-440. 本文二维码信息
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QuEChERS-气相色谱-串联质谱法测定鸡蛋中氟虫腈及其代谢产物
Determination of fipronil and its metabolites in eggs by QuEChERS-gas chromatography-tandem mass spectrometry
投稿时间:2019-09-05  
DOI:
中文关键词:  鸡蛋  分散固相萃取  氟虫腈及其代谢产物  气相色谱-串联质谱
Key Words:Egg  dispersive solid phase extraction  fipronil and its metabolites  gas chromatography-tandem mass spectrometry
基金项目:佛山市卫生和计划生育局医学科研项目(20190208)
作者单位E-mail
兰红军 广东省佛山市南海区疾病预防控制中心,广东 佛山 528200 359820312@qq.com 
吴雪梅 广东省佛山市南海区疾病预防控制中心,广东 佛山 528200  
冯耀基 广东省佛山市南海区疾病预防控制中心,广东 佛山 528200  
黎少映 广东省佛山市南海区疾病预防控制中心,广东 佛山 528200  
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中文摘要:
      目的 建立QuEChERS-气相色谱-串联质谱同时测定鸡蛋中氟虫腈及其代谢产物的方法。方法 于5.0 g鸡蛋样品中加入3 ml水,加入10 ml乙腈提取,提取液经EMR-Lipids管净化。采用DB-5MS(30 m×0.25 mm,0.25 μm)进行分离,多反应监测(MRM)模式进行检测,基质匹配曲线外标法定量。结果 氟虫腈及其代谢产物在0~60 μg/L范围内线性良好,相关系数(r)均≥0.999 0,检出限(S/N=3)为0.5~0.8 μg/kg,定量限(S/N=10)为1.7~2.7 μg/kg。回收率为92.0%~115.5%,相对标准偏差(RSD)为3.6%~6.8%(n=6)。结论 该方法具有前处理方法简单、灵敏度高、回收率高等特点,适用于鸡蛋中氟虫腈及其代谢产物的准确检测。
Abstract:
      Objective To establish a method for the simultaneous determination of fipronil and its metabolites in eggs by QuEChERS-gas chromatography-tandem mass spectrometry. Methods 3 ml water was added into egg samples (5.0 g), extracted with 10 ml acetonitrile, and purified in an EMR-Lipids tube. The analytes were performed on DB-5MS column (30 m×0.25 mm, 0.25 μm), detected under multiple reaction monitoring (MRM) mode, and was quantified by external standard method with matrix matching curve. Results The fipronil and its metabolites had a good linear in the range of 0-60 μg/L with the correlation coefficient r≥0.999 0. The detection limits (S/N=3) were 0.5-0.8 μg/kg, and the limits of quantification (S/N=10) were 1.7-2.7 μg/kg. The recoveries were 92.0%-115.5%, and the relative standard deviation (RSD) were 3.6%-6.8% (n=6). Conclusion The method has the characteristics of simple pretreatment, high sensitivity and high recoveries, and it is suitable for the accurate determination of fipronil and its metabolites in eggs.
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