Shen Weijian, Liu Han, Zhang Rui, Yu Keyao, Cai Lisheng, Liu Yan, Wang Hong
Food Laboratory of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210019, China.
Se Pu. 2017 Dec 8;35(12):1224-1228. doi: 10.3724/SP.J.1123.2017.09033.
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 metabolites in eggs and egg products.
建立了一种采用气相色谱-负化学电离-质谱联用(GC-NCI-MS)测定鸡蛋和蛋制品中氟虫腈及其代谢物的方法。目标物用乙腈从样品中提取,然后通过一种称为分散固相萃取QuEChERS的简单净化步骤进行处理。提取物采用GC-NCI-MS测定,并通过外标法和基质校正标准曲线进行定量。在四个加标水平(0.1、2.0、4.0和20.0 μg/kg)下,回收率在87.0%至99.3%之间,四种分析物的相对标准偏差均不超过12.7%。该方法在0.005至0.10 mg/L之间线性良好,所有定量限均小于0.10 μg/kg。因此,该方法可用于测定鸡蛋和蛋制品中氟虫腈及其代谢物的残留量。