超高效液相色谱-串联质谱法测定鲜鸡蛋中氟虫腈及其代谢物残留

Determination of fipronil and its metabolites in fresh eggs by ultra high performance liquid chromatography-tandem mass spectrometry

采用优化的QuEChERS前处理方法,并结合超高效液相色谱-串联质谱法对鲜鸡蛋中氟虫腈及其代谢物残留进行测定,并对该方法的线性、灵敏度、回收率及基质效应等进行验证,同时对市场采集的鲜鸡蛋样品开展筛查分析。试验结果表明,氟虫腈及其3种代谢物在1.0~100μg·L^-1范围内呈线性,相关系数(R2)均大于0.99。不同浓度加标回收试验所得回收率为85.8%~105.6%,相对标准偏差均小于11.0%,基质效应为0.88~1.23。氟虫腈及其3种代谢物在该方法中最低检出限为0.002~0.02μg·kg^-1,定量限为0.007~0.05μg·kg^-1。通过对30批次鲜鸡蛋样品的检测分析,其中1批次检出氟虫腈,残留含量为10.1μg·kg^-1。

The optimized QuEChERS method combined with ultra-high performance liquid chromatography-tandem mass spectrometry was developed to determine fipronil and its metabolite residues in fresh eggs.The linearity,sensitivity,recovery rate and matrix effect of the method were verified.Meanwhile,the screening analysis for fipronil and its metabolite residues in fresh eggs collected from the market was carried out.The results showed that the linearity of fipronil and its three metabolites were in the range of 1.0-100μg·L^-1,and the correlation coefficient(R2)was greater than 0.99,the recoveries were 85.8%-105.6%,the relative standard deviation was less than 11.0%,and the matrix effect was 0.88-1.23.The detection limit for fipronil and its metabolite were 0.002-0.02μg·kg^-1,and the limit of quantification(LOQ)was 0.007-0.05μg·kg^-1.The developed method was used to analyze 30 batches of fresh egg samples,and the results showed that fipronil was detected in one sample with the concentration of 10.1μg·kg^-1.