A first approach using micellar electrokinetic capillary chromatography for the determination of fipronil and fipronil‐sulfone in eggs
A first approach using micellar electrokinetic capillary chromatography for the determination of fipronil and fipronil‐sulfone in eggs
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DOI：
10.1002/elps.201900291
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发表时间：
2019-11
期刊：
影响因子：
2.9
通讯作者：
M. Aparicio-Muriana;I. Lhotská;A. García-Campaña;Francisco J. Lara
中科院分区：
文献类型：
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作者：
M. Aparicio-Muriana;I. Lhotská;A. García-Campaña;Francisco J. Lara
氟虫腈是一种杀虫剂，在欧盟未被批准用于食品。2017年，由于在家禽养殖场中非法使用，氟虫腈存在于新鲜鸡蛋中，因此需要可靠的方法来确定这些基质中的氟虫腈及其主要代谢产物。在这项工作中，我们报告了通过CE研究非泼罗尼和两种代谢产物非泼罗尼-砜和非泼罗尼-硫化物的第一种方法。采用MEKC模式，使用50 mM全氟辛酸铵（pH 9.0）和10%（v/v）甲醇的溶液作为背景电解质。将拟定方法与基于盐析辅助液液萃取（SALLE）的简单样品处理相结合，使用乙腈作为萃取溶剂，硫酸铵作为盐。SALLE-MEKC-UV法可同时定量非泼罗尼和非泼罗尼砜。验证参数得到了令人满意的结果，精密度，表示为相对标准偏差，低于14%，回收率高于83%。非泼罗尼的检测限为90 µg/kg，非泼罗尼-砜的检测限为150 µg/kg，因此在灵敏度方面，需要进一步研究允许额外预浓缩的样品处理或使用更灵敏的检测，如MS。
Fipronil is an insecticide that is not approved in the European Union in food. In 2017, fipronil was involved in a European health alert due to its presence in fresh hen eggs because of an illicit use in poultry farms, so reliable methods are needed to determine fipronil and its main metabolites in these matrixes. In this work, we report the first approach to the study of fipronil and two metabolites, fipronil‐sulfone and fipronil‐sulfide by CE. MEKC mode was employed using a solution of 50 mM ammonium perfluorooctanoate pH 9.0 with 10% (v/v) methanol as background electrolyte. The proposed method was combined with a simple sample treatment based on salting‐out assisted LLE (SALLE) using acetonitrile as extraction solvent and ammonium sulfate as salt. The SALLE–MEKC–UV method allowed the simultaneous quantification of fipronil and fipronil‐sulfone. Validation parameters yielded satisfactory results, with precision, expressed as relative SD, below 14% and recoveries higher than 83%. Limits of detection were 90 µg/kg for fipronil and 150 µg/kg for fipronil‐sulfone, so in terms of sensitivity further studies of sample treatments allowing extra preconcentration or the use of more sensitive detection, such as MS, would be needed.