A method was established for the determination of fipronil and its metabolites in eggs and egg products with gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS). The targets were extracted from samples with acetonitrile,and followed by a simple cleanup step known as dispersive solid-phase extraction QuEChERS. The extracts were determined by GC-NCI-MS,and quantified by external standard method with matrix correction standard curves. The recoveries were in the range of 87. 0% to 99. 3% at four spiked levels ( 0. 1,2. 0,4. 0 and 20. 0 μg/kg),and all RSDs were not more than 12. 7% for the four analytes. The linearity of the method was good between 0. 005 and 0. 10 mg/L,and all LOQs were less than 0. 10 μg/kg. So this method can be used to determine the residues of fipronil and its me-tabolites in eggs and egg products.%建立了气相色谱-负化学源质谱联用技术(GC-NCI-MS)测定禽蛋及蛋制品中氟虫腈及其3种代谢物残留量的方法.样品经乙腈提取,分散固相萃取技术QuEChERS净化,采用基质校正曲线外标法定量.在0.005~0.10 mg/L范围内氟虫腈及其3种代谢物均呈现良好的线性关系,所有目标物的定量限均在0.025~0.10μg/kg范围内,均能满足国内外的限量要求.在0.1、2.0、4.0、20.0μg/kg 4个添加水平下,氟虫腈及其3种代谢物的平均回收率均处于87.0%~99.3%,RSD均≤12.7%,说明该法有较高的准确度和较好的稳定性.综上所述,该法灵敏度、准确度较高,精密度较好,可用于禽蛋及蛋制品中氟虫腈及其代谢物残留量的测定.
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