GC-MS快速测定鲜蛋中氟虫腈及其代谢物

Rapid Determination of Fipronil and Its Metabolites in Fresh Eggs by GC-MS

采用气相色谱-质谱法快速测定鲜蛋中氟虫腈及其三种代谢物的含量。鲜蛋样品经酸化乙腈提取后,经固相萃取柱(石墨化炭黑-氨基复合柱)净化,用GC-MS测定,内标法定量。结果表明,氟虫腈及其代谢物在20~1 000μg/L范围内呈较好的线性关系,线性相关系数(R^2)均大于0.998,检出限在4.2~8.5μg/kg之间,氟虫腈及其代谢物在3个添加水平(5, 10和50μg/kg)下回收率为71.3%~116.3%,相对标准偏差(RSD, n=6)为1.5%~8.9%,该方法简单、快速,满足现行国家标准对鸡蛋中氟虫腈及其代谢物的残留检测限量的要求。

The contents of fipronil and its three metabolites in fresh eggs were determined by gas chromatography-mass spectrometry. The samples were extracted by acidified acetonitrile, purified by solid phase extraction column(graphitized carbon black-amino composite column), determined by GC-MS, and quantified by internal standard method. The results showed that the linearity of fipronil and its metabolites was good in the range of 20-1 000 μg/L with correlation coefficients(R^2) which were more than 0.998. The detection limit was 4.2-8.5 μg/kg. The recovery of fipronil and its metabolites was 71.3%-116.3% at three levels(5, 10 and 50 μg/kg). The relative standard deviation(RSD, n=6) was 1.5%-8.9%. The method was simple and rapid, and it met the requirements of current countries standard requirements for detection limits of fipronil and its metabolites residues in eggs.