Determinación de fipronil y su principal metabolito en muestras de origen animal mediante cromatografía de líquidos acoplada a espectrometría de masas en tandem
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2024-01-09
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Jaén: Universidad de Jaén
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Desde el verano de 2017 en el Sistema Europeo de Alertas para Alimentos y
Piensos (Rapid Alert System for Food and Feed-European Commission: RASFF)
se ha visto un considerable incremento de notificaciones respecto a la presencia
de fipronil en huevos y carne de ave. La primera alerta que se detectó en Julio,
fue en Bélgica y la decisión de riesgo fue seria. Tras esta alerta no han parado
de detectar este plaguicida, forma parte del grupo de los insecticidas y que se
utiliza principalmente para plagas de insectos. Tras Bélgica fue Luxemburgo,
Noruega, Holanda, Hungría, Italia, Eslovaquia, Malta, Alemania, Polonia,
República Checa, Gracia, Austria y por último Francia. En esta última la alerta
es de huevos procedentes de España. Puesto de manifiesto este problema, en
este trabajo se ha desarrollado una metodología para la detección del fipronil y
su principal metabolito en huevos de gallina. De tal forma que no solo se
identifique, sino que se cuantifique para comprobar que se cumplen los límites
permitidos en este tipo de matrices alimentarias. Para la detección se empleó la
cromatografía líquida de alta resolución acoplada a un espectrómetro de masas
en tándem (UHPLC-MS/MS) con un triple cuadrupolo (QqQ) como analizador
equipado con una fuente de ionización electrospray (ESI) operando en modo
negativo. La identificación del fipronil y de su metabolito: fipronil sulfona, se llevó
a cabo a partir de la medida de las transiciones ion precursor/ión producto
características para cada compuesto y del tiempo de retención. Por otra parte,
se han evaluado tres tratamientos de muestra: (i) extracción en fase sólida con
cartuchos Oasis HLB PRiME (Hidrophilic-lipophilic balance) (Process
Robustness improvements in Matrix Easy of use); (ii) extracción en fase sólida
dispersiva, se conoce por su acrónimo en inglés: “QuEChERS” que significa,
Quick, Easy, Cheap, Effective, Rugged y Safe; utilizando como sorbente
Enhanced Matrix Removal -lipid (EMR-lipid) y; (iii) QuEChERS utilizando como
sorbente Amina Primaria Secundaria (PSA). Una vez, puesta a punto la
metodología, ésta finalmente se ha aplicado a 9 muestras de huevo de diferentes
marcas comerciales, obtenidas en supermercados de la localidad.
The European Food and Safety Alerts System (RASFF) has increased the number notifications about the presence of fipronil in eggs and poultry meat since the last summer. The first notified alert detected was in July from Belgium. RASFF considered the risk as serious. Then, the number of notifications has been growing continuously, due to this compound is widely use as insecticide to kill, harm, repel or mitigate one or more species of insect. In the last year, more cases have been notified in different countries including Luxembourg, Norway, Holland, Hungary, Italy, Slovakia, Malta, Germany, Poland, Czech Republic, Grace, Austria and France. The last came from Spain. The decision of risk of all these alerts is not serious, since the concentration of the pesticide does not the dangerous for the human being. Bearing in mind this problem, in this work a new A Ultra High-resolution liquid chromatography coupled to a tandem mass spectrometer (UHPLC-MS/MS) method has been developed for the determination of fipronil and its main metabolite in chicken eggs. So, the residue is not only identified, but also it is quantified to verify that the limits allowed in this type of food matrices are fulfil. The identification of fipronil and its metabolite: fipronil sulfone, was carried out from the mass of de ions of interest and retention time. In addition, three sample treatment procedures have been evaluated: (i) solid-phase extraction using Oasis HLB PRiME (Hydrophilic-lipophilic balanced, Process Robustness improvements in Matrix Easy of use); and QuEChERS (means, Quick, Easy, Cheap, Effective, Rugged and Safe) using as dispersive solid phase extraction sorbent (ii) Enhanced Matrix Removal-lipid (EMR-lipid) or (iii) Primary amine (PSA). Finally, 9 samples of eggs of different commercial brands, obtained in local supermarkets, were analyzed to check the presence of this pesticide.
The European Food and Safety Alerts System (RASFF) has increased the number notifications about the presence of fipronil in eggs and poultry meat since the last summer. The first notified alert detected was in July from Belgium. RASFF considered the risk as serious. Then, the number of notifications has been growing continuously, due to this compound is widely use as insecticide to kill, harm, repel or mitigate one or more species of insect. In the last year, more cases have been notified in different countries including Luxembourg, Norway, Holland, Hungary, Italy, Slovakia, Malta, Germany, Poland, Czech Republic, Grace, Austria and France. The last came from Spain. The decision of risk of all these alerts is not serious, since the concentration of the pesticide does not the dangerous for the human being. Bearing in mind this problem, in this work a new A Ultra High-resolution liquid chromatography coupled to a tandem mass spectrometer (UHPLC-MS/MS) method has been developed for the determination of fipronil and its main metabolite in chicken eggs. So, the residue is not only identified, but also it is quantified to verify that the limits allowed in this type of food matrices are fulfil. The identification of fipronil and its metabolite: fipronil sulfone, was carried out from the mass of de ions of interest and retention time. In addition, three sample treatment procedures have been evaluated: (i) solid-phase extraction using Oasis HLB PRiME (Hydrophilic-lipophilic balanced, Process Robustness improvements in Matrix Easy of use); and QuEChERS (means, Quick, Easy, Cheap, Effective, Rugged and Safe) using as dispersive solid phase extraction sorbent (ii) Enhanced Matrix Removal-lipid (EMR-lipid) or (iii) Primary amine (PSA). Finally, 9 samples of eggs of different commercial brands, obtained in local supermarkets, were analyzed to check the presence of this pesticide.