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鸡蛋中的氟虫腈。LC-MS/MS 是唯一的选择吗?LC-MS/MS 和 GC-ECD 分析氟虫腈的比较研究。

Fipronil in eggs. Is LC-MS/MS the only option? A comparison study of LC-MS/MS and GC-ECD for the analysis of fipronil.

机构信息

National Reference Laboratory of Pesticides Residues, Department of Pesticides Control and Phytopharmacy, Benaki Phytopathological Institute, St. Delta 8 str., 14561 Kifissia, Greece.

National Reference Laboratory of Pesticides Residues, Department of Pesticides Control and Phytopharmacy, Benaki Phytopathological Institute, St. Delta 8 str., 14561 Kifissia, Greece.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Oct 15;1129:121785. doi: 10.1016/j.jchromb.2019.121785. Epub 2019 Sep 7.

DOI:10.1016/j.jchromb.2019.121785
PMID:31677523
Abstract

Fipronil is a broad-spectrum insecticide belonging to the phenylpyrazole chemical family, classified by the U.S. EPA as a group C (possible human) carcinogen. It is highly toxic to crustaceans, insects and zooplankton as well as to termites, rabbits and certain groups of gallinaceous birds. In European Union and Greece, fipronil is authorized only for the control of termites and cockroaches and not as a plant protection product or as a veterinary drug. The definition of residue of fipronil comprises of the sum of fipronil and its sulfone metabolite expressed as fipronil and is set at 5 μg kg. In this study, a sensitive and reliable modified QuEChERS method, proposed by the European Reference Laboratory for animal origin products, has been validated and applied to the residue analysis of fipronil and its metabolites (sulfone and desulfinyl) in chicken eggs and other egg products by LC-MS/MS and GC-ECD analysis. The two analytical systems performed almost equally concerning validation process and with regard to the analysis of real samples, results from both systems were in agreement: out of 11 samples analysed, 4 samples showed measurable residues of fipronil sulfone with 3 samples exceeding the MRL limit.

摘要

氟虫腈是一种属于苯并吡唑类化学家族的广谱杀虫剂,被美国环保署归类为 C 类(可能对人类)致癌物。它对甲壳类动物、昆虫和浮游动物以及白蚁、兔子和某些家禽鸟类具有高度毒性。在欧盟和希腊,氟虫腈仅被授权用于控制白蚁和蟑螂,而不作为植物保护产品或兽药使用。氟虫腈残留的定义包括氟虫腈及其砜代谢物的总和,以氟虫腈表示,设定为 5μg/kg。在这项研究中,采用了由动物源产品欧洲参考实验室提出的一种灵敏可靠的改良 QuEChERS 方法,通过 LC-MS/MS 和 GC-ECD 分析,对鸡蛋和其他蛋制品中氟虫腈及其代谢物(砜和脱磺酰基)的残留进行了验证和应用。这两个分析系统在验证过程中表现几乎相同,并且在分析实际样品时,两个系统的结果一致:在所分析的 11 个样品中,有 4 个样品显示出可测量的氟虫腈砜残留,其中 3 个样品超过了 MRL 限量。

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