Food Safety Laboratory, Division of Metrology in Chemistry, National Institute of Metrology, Beijing 100029, China.
Food Safety Laboratory, Division of Metrology in Chemistry, National Institute of Metrology, Beijing 100029, China.
Food Chem. 2019 May 30;281:85-90. doi: 10.1016/j.foodchem.2018.12.041. Epub 2018 Dec 17.
Fipronil is a highly toxic insecticide, and fipronil egg scandal greatly threaten people's health. Herein, a precise and reliable method was developed for the determination of fipronil and three metabolites in chicken egg by GC-EI-MS. Sample pretreatment took about 20 min and baseline separation of four analytes were realized within 12 min by GC-MS. Moreover, the limits of detection were 0.2-0.5 ng g and the limits of quantitation was 0.5-1 ng g with relative standard deviations (RSDs) lower that 3.32%. Satisfactory recoveries were get in the range of 81.16-103.57% for three levels of spiked samples. Finally, the developed method has been applied for the analysis of egg samples from four sources. Results showed that fipronil and fipronil-sulfone were detected in three samples, while fipronil-desulfinyl and fipronil-sulfide were totally absent. The method showed great promising in quantification of fipronil and its metabolites in food safety affairs.
氟虫腈是一种剧毒杀虫剂，氟虫腈鸡蛋事件极大地威胁了人们的健康。本研究建立了一种通过 GC-EI-MS 检测鸡蛋中氟虫腈及其三种代谢物的准确可靠的方法。样品预处理耗时约 20 分钟，通过 GC-MS 可在 12 分钟内实现四种分析物的基线分离。此外，检测限为 0.2-0.5ng/g，定量限为 0.5-1ng/g，相对标准偏差（RSD）低于 3.32%。三种加标水平的样品回收率均在 81.16-103.57%之间。最后，该方法已应用于四种来源的鸡蛋样品分析。结果表明，三种样品中检测到氟虫腈和氟虫腈砜，而氟虫腈去磺隆和氟虫腈硫醚则完全不存在。该方法在食品安全事务中对氟虫腈及其代谢物的定量检测具有广阔的应用前景。
