气相色谱三重四极杆串联质谱法测定鸡蛋和鸡肉中氟虫腈及其代谢物残留量的研究

Determination of residues of fipronil and its metabolite in eggs and chicken by gas chromatography-tandem mass spectrometry

中文关键词:  氟虫腈及其代谢物  农药残留  气相色谱三重四级杆串联质谱法  鸡蛋和鸡肉  

英文关键词:fipronil and metabolite  Spesticide residue  gas chromatography-tandem mass spectrometry  Chicken egg and muscle

中文摘要:

      目的 建立一种鸡蛋和鸡肉组织中氟虫腈及其代谢物的农药残留的气相色谱-串联质谱法(GC-MS/MS)检测方法。方法 样品经乙腈提取,Bond Elut EMR-Lipids 法净化,去除鸡肉和鸡蛋组织中的脂类和蛋白质。质谱采用多离子检测模式(MRM)对氟虫腈及其代谢物的定量离子和定性离子进行监测。结果 本方法中氟虫腈及其代谢物在20.0~1000μg/L的浓度范围内,线性良好,相关系数 r₂ 大于0.994,在20、50、100μg/L水平上的平均回收率在91～114.32%之间,相对标准偏差RSD为0.4～7.8% (n=6),氟虫腈及其代谢物的定量限(S/N=10)为1.9～4.8μg/kg。结论 该方法具有前处理简便快捷、净化效果佳、灵敏度高、成本低等特点,适用于农产品鸡蛋和鸡肉中氟虫腈的快速确认及定量检测。

英文摘要:

      Objective To establish a sensitive and reliable method for determination of residues of fipronil and its metabolite in eggs and chicken by gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods Eggs and chicken samples were extracted with acetronitrile, and cleaned-up by Bond Elut EMR-Lipids, which could remove fat and protein from eggs and chicken. The purged liquor were determined by GC–MS/MS under multiple reaction monitoring (MRM) for monitoring the quantitative and qualitative ions of fluoridinitrile and its metabolites. Results The fluonitrile and its metaboliteshad good linearity in the concentration range of 20.0-1000 μg/L and the correlation coefficient (r2) were higher than 0.994. The average recoveries of fipronil and metabolite were 91%-114.32% at the spiked levels of 10, 20, 50 μg/L, with the relative standard deviations (RSDs) of 0.4%-7.8%. The limit of detection (LOD) (S/N=3) for fipronil and its metabolite in eggs and chicken samples were 2.0-3.5 μg/kg, the limits of quantification (LOQ) (S/N=10) were 6.0-10.5 μg/kg. Conclusion This method has advantages of simple pretreatment, good purification effect, high sensitivity and low cost, which is suitable for the rapid confirmation and quantitative detection of fluronitrile in eggs and chicken.