Development of a simple method to quantify fipronil and its intermediates in soil.

Autor: Tomazini R; Laboratory of Environmental Biogeochemistry, Nucleus of Diagnoses and Environmental Interventions, Department of Chemistry, Federal University of São Carlos - UFSCar, Via Washington Luís km 235, São Carlos 13565-905, SP, Brazil. rftmazini@gmail.com guilhermegrosseli@gmail.com dnrsousa@yahoo.com.br psfadini@ufscar.br amozeto@ufscar.br., Grosseli GM; Laboratory of Environmental Biogeochemistry, Nucleus of Diagnoses and Environmental Interventions, Department of Chemistry, Federal University of São Carlos - UFSCar, Via Washington Luís km 235, São Carlos 13565-905, SP, Brazil. rftmazini@gmail.com guilhermegrosseli@gmail.com dnrsousa@yahoo.com.br psfadini@ufscar.br amozeto@ufscar.br., Nara Ribeiro de Sousa D; Laboratory of Environmental Biogeochemistry, Nucleus of Diagnoses and Environmental Interventions, Department of Chemistry, Federal University of São Carlos - UFSCar, Via Washington Luís km 235, São Carlos 13565-905, SP, Brazil. rftmazini@gmail.com guilhermegrosseli@gmail.com dnrsousa@yahoo.com.br psfadini@ufscar.br amozeto@ufscar.br., Fadini PS; Laboratory of Environmental Biogeochemistry, Nucleus of Diagnoses and Environmental Interventions, Department of Chemistry, Federal University of São Carlos - UFSCar, Via Washington Luís km 235, São Carlos 13565-905, SP, Brazil. rftmazini@gmail.com guilhermegrosseli@gmail.com dnrsousa@yahoo.com.br psfadini@ufscar.br amozeto@ufscar.br., Talarico Saia F; Institute of Marine Sciences, Federal University of São Paulo, Av. Dr Carvalho de Mendonça, 144, Encruzilhada, 11070-102, Santos, SP, Brazil. ftsaia@yahoo.com.br., Langenhoff A; Department of Environmental Technology, Wageningen University & Research, PO Box 17, 6700 EV Wageningen, The Netherlands. alette.langenhoff@wur.nl., van der Zaan B; Subsurface and Groundwater Systems Deltares, PO Box 85467, 3508 AL, Utrecht, The Netherlands. bas.vanderZaan@deltares.nl., Mozeto AA; Laboratory of Environmental Biogeochemistry, Nucleus of Diagnoses and Environmental Interventions, Department of Chemistry, Federal University of São Carlos - UFSCar, Via Washington Luís km 235, São Carlos 13565-905, SP, Brazil. rftmazini@gmail.com guilhermegrosseli@gmail.com dnrsousa@yahoo.com.br psfadini@ufscar.br amozeto@ufscar.br.
Jazyk: angličtina
Zdroj: Analytical methods : advancing methods and applications [Anal Methods] 2020 Jul 02; Vol. 12 (25), pp. 3242-3249.
DOI: 10.1039/d0ay00924e
Abstrakt: A simple and reproducible method was developed and validated for simultaneous quantification of the pesticide fipronil and its intermediates fipronil desulfinyl, fipronil sulfone and fipronil sulfide, in soil. The analytes were extracted by ultrasonic bath and the ratio of solvents (hexane/acetone), number and time of cycles were optimized by Box-Behnken design with a triplicate central point. The optimal extraction conditions were achieved through a response surface analysis. The clean-up step was conducted by cartridges of solid phase extraction (SPE) containing silica (Florisil®) and aluminum oxide. Gas chromatography with electron capture detection (GC-ECD) was employed for separating fipronil and its intermediates with a suitable resolution and runtime of 20 minutes. The best quantification was achieved with 1 : 1 (v/v) acetone/hexane and 2 ultrasound cycles of 15 minutes each. The recovery values were between 81 to 108%, with relative standard deviation (RSD) lower than 6%, with no effect of the used matrix. Analytical curves presented regression coefficients values above 0.9908 for a concentration range from 0.005 to 0.6 μg g-1. Limits of detection (LOD) from 0.002 to 0.006 μg g-1 and limits of quantification (LOQ) from 0.006 to 0.020 μg g-1 were reached for all analytes. This method can be used to monitor and quantify fipronil and its intermediates in soil.
Databáze: MEDLINE