超高效液相色谱-串联质谱法测定腌鱼中氟虫腈及其代谢物的残留

Determination of Fipronil and Its Metabolites Residues in Salted Fish by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

本文采用超高效液相色谱串联质谱法测定了腌鱼中氟虫腈及其代谢物氟虫腈砜、氟虫腈亚砜、氟甲腈。腌鱼样品经乙腈提取、盐析和吸附剂净化,以0.1%甲酸的甲醇溶液和0.1%甲酸的5 mmoL·L^(-1)乙酸铵溶液为淋洗液在BEH C18色谱柱梯度洗脱,电喷雾负离子多反应监测(Multiple Reaction Monitoring,MRM)模式检测。结果表明,氟虫腈及其代谢物在0.25~10.0 ng·mL^(-1)呈良好的线性关系,相关系数均大于0.999;在1.0~10.0μg·kg^(-1)添加范围内,氟虫腈及其代谢物的回收率为91.79%~109.84%,相对标准偏差为0.91%~3.39%(n=6);该方法检出限和定量限分别为0.2~0.4μg·kg^(-1)和0.8~1.2μg·kg^(-1)。本方法操作简单、灵敏,可同时测定腌鱼中氟虫腈及其代谢物的残留量,为其日常监管提供技术参考。

The fipronil and its metabolites fipronil sulfone,fipronil sulfoxide and fipronil in pickled fish were determined by ultra high performance liquid chromatography tandem mass spectrometry in this paper.The samples of pickled fish were extracted by acetonitrile,dehydrated and purified by adsorbent.0.1%formic acid in methanol solution and 0.1%formic acid in 5 mmoL·L^(-1)ammonium acetate solution were eluted on a BEH C18 column in gradient elution mode,electrospray anion multiple reaction monitoring mode detection.The results showed that there was a good linear relationship between fipronil and its metabolites in the range of 0.25~10.00 ng·mL^(-1),and the correlation coefficients were all greater than 0.999;The recovery rate of fipronil and its metabolites within the addition range of 1.0~10.0μg·kg^(-1)were 91.79%~109.84%,the relative standard deviations were 0.91%~3.39%(n=6);The limits of detection and quantification of the method were 0.2~0.4μg·kg^(-1)and 0.8~1.2μg·kg^(-1).The method is simple,sensitive,and can simultaneously determine the residues of fifionil and its metabolites in salted fish,so as to provide technical reference for daily supervision.