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Development and Validation of an Analytical Method to Determine Fipronil and its Degradation Products in Soil Samples

Abstract

The aim of this study was to develop a methodology for identifying and quantifying Fipronil and its degradation products in soil by gas chromatography–electron capture detector previously extracted using a focused ultrasound probe. This methodology was obtaining a range of recovery between 85 % and 120 %, decreasing approximately solvent used time and cost, respect to other methodologies such as bath ultrasonic, solid-phase extraction, liquid–liquid extraction and soxhlet. The method was validated in fortified matrix, presented linearity in the range of 25–400 μg kg−1, and limit of detection for Fipronil and their products desulfinyl, sulfide and sulfone was 14.7, 9.8, 8.9 and 10.7 μg kg−1, respectively. This process was applied to samples of agricultural soils, where two degradation products desulfinyl and sulfone were found.

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Acknowledgments

R Flores-Ramirez was supported by a fellowship from CONSEJO NACIONAL DE CIENCIA Y TECNOLOGÍA (CONACyT #20122).

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Correspondence to R. Flores-Ramírez.

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Flores-Ramírez, R., Batres-Esquivel, L.E., Díaz-Barriga Martínez, F. et al. Development and Validation of an Analytical Method to Determine Fipronil and its Degradation Products in Soil Samples. Bull Environ Contam Toxicol 89, 744–750 (2012). https://doi.org/10.1007/s00128-012-0780-y

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Keywords

  • Fipronil
  • Degradation products
  • GC–ECD
  • Focused ultrasound probe