RESUMEN
To response to the need for a rapid, cost-effective, eco-friendly and efficient extraction process, a sensitive method for the determination of ethylenethiourea (ETU) in food matrices by high-performance liquid chromatography-mass spectrometry (HPLC-LC/MS) was developed and validated. ETU was extracted from food commodities with methanol, cleaned up by alumina-SPE column, and then determined by HPLC-MS/MS. The MS detection was operated in positive ionization mode. For confirmation of target compound, two precursor ion>product ion transitions were selected by multi-reaction monitoring mode (MRM). The method showed good linearity with correlation coefficient higher than 0.9950. Recoveries at three spiked levels (10, 50, 100 ng/g) in random selected food matrices were in range of 71-121% with RSDs not larger than 25%. The limit of quantitation for the analyte was estimated at 5 ng/g.
Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Etilenotiourea/análisis , Etilenotiourea/aislamiento & purificación , Contaminación de Alimentos/análisis , Fungicidas Industriales/análisis , Extracción en Fase Sólida/métodos , Espectrometría de Masas en Tándem/métodos , Análisis de los AlimentosRESUMEN
A rapid and sensitive analytical method for the determination of ethylenethiourea (ETU) in potatoes and cucumbers is developed. This method employs modified QuEChERS followed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) analysis. ETU was extracted by alkaline acetonitrile (containing 1%NH(3).H(2)0), separated on a ZIC-pHILIC column, confirmed by multiple reaction monitoring (MRM) mode with electrospray ionisation source. This modified procedure showed satisfactory recovery (90.6-103.5%) fortified at the range of 0.005-0.05 mg kg(-1) with relative standard deviation (RSD)<7%. The limits of detection (LOD) and the limits of quantification (LOQ) were 0.002 mg kg(-1) and 0.005 mg kg(-1), respectively. Matrix effect and HILIC retention mechanism were also evaluated. The method was finally applied to detect ETU in potato and cucumber samples collected at harvest period. Residues of ETU were detected in four cucumber samples with the level lower than LOQ.
Asunto(s)
Cucumis sativus/química , Etilenotiourea/análisis , Etilenotiourea/aislamiento & purificación , Fungicidas Industriales/análisis , Fungicidas Industriales/aislamiento & purificación , Solanum tuberosum/química , Extracción en Fase Sólida/métodos , Cromatografía Líquida de Alta Presión/métodos , Contaminación de Alimentos/análisis , Límite de Detección , Residuos de Plaguicidas/análisis , Residuos de Plaguicidas/aislamiento & purificación , Espectrometría de Masas en Tándem/métodosRESUMEN
Laboratory studies were conducted in a model system to determine the effects of ozone (1 and 3 ppm) and hydrogen peroxyacetic acid (HPA) (5 and 50 ppm) at pH 4.6, 7.0, and 10.7 and at 10 and 21 degrees C on the degradation of mancozeb in solution over a 30 min period. All samples were analyzed for residues by GLC and HPLC. Ozonation and HPA treatment were effective in degrading mancozeb in solution. Rate of mancozeb degradation was dependent on pH, with the fastest rate at pH 7.0. Ethylenethiourea (ETU) residue concentrations in the mancozeb solutions were monitored over 60 min. Under controlled conditions, the ETU residue concentrations increased during the 15 min reaction time and then decreased for all three pH values. At 3 ppm of ozone treatment, no ETU residues were detected at all three pH ranges after 15 min of reaction time. Degradation of ETU by HPA was greatest at pH 4.6, and no ETU residues remained after 5 min at either 5 or 50 ppm. The results showed that ozone and HPA gave excellent degradation of pesticide residues depending on pH and temperature. These experiments indicated the potential for the removal of pesticide residues on fruit and in processed products.