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A first approach using micellar electrokinetic capillary chromatography for the determination of fipronil and fipronil-sulfone in eggs
MM. Aparicio-Muriana, I. Lhotská, AM. García-Campaña, FJ. Lara
Language English Country Germany
Document type Journal Article, Research Support, Non-U.S. Gov't
Grant support
CZ.02.1.01/0.0/0.0/15_003/0000465
European Regional Development Fund - International
FPU17/03810
Ministerio de Ciencia, Innovación y Universidades - International
AGL2015-70708-R
Secretaría de Estado de Investigación, Desarrollo e Innovación - International
2013/2
Universidad de Granada - International
- MeSH
- Acetonitriles MeSH
- Chromatography, Micellar Electrokinetic Capillary methods MeSH
- Insecticides MeSH
- Chickens MeSH
- Limit of Detection MeSH
- Linear Models MeSH
- Pyrazoles analysis MeSH
- Reproducibility of Results MeSH
- Eggs analysis MeSH
- Animals MeSH
- Check Tag
- Animals MeSH
- Publication type
- Journal Article MeSH
- Research Support, Non-U.S. Gov't MeSH
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.
References provided by Crossref.org
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- $a 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.
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