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

Author(s)

Tomazini, Rafaela ^[1] ; Grosseli, Guilherme Martins ^[1] ; Ribeiro de Sousa, Diana Nara ^[1] ; Fadini, Pedro Sergio ^[1] ; Saia, Flavia Talarico ^[2] ; Langenhoff, Alette ^[3] ; van der Zaan, Bas ^[4] ; Mozeto, Antonio Aparecido ^[1]

Affiliation

^[1] Fed Univ Sao Carlos UFSCar, Dept Chem, Lab Environm Biogeochem Nucleus Diagnoses & Envir, Via Washington Luis Km 235, BR-13565905 Sao Carlos, SP - Brazil

^[2] Univ Fed Sao Paulo, Inst Marine Sci, Av Dr Carvalho de Mendonca 144, BR-11070102 Santos, SP - Brazil

^[3] Wageningen Univ & Res, Dept Environm Technol, POB 17, NL-6700 EV Wageningen - Netherlands

^[4] Subsurface & Groundwater Syst Deltares, POB 85467, NL-3508 AL Utrecht - Netherlands

• Document type: Journal article
• Source: ANALYTICAL METHODS; v. 12, n. 25, p. 3242-3249, JUL 7 2020.
• Web of Science Citations: 0

Abstract

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 (R)) 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 mu g g(-1). Limits of detection (LOD) from 0.002 to 0.006 mu g g(-1)and limits of quantification (LOQ) from 0.006 to 0.020 mu g g(-1)were reached for all analytes. This method can be used to monitor and quantify fipronil and its intermediates in soil. (AU)

• FAPESP's process: 12/51496-3 - The environmental impact of biofuel production: functional bio-indicators for sustainable and optimal biofuel production
• Grantee: Flávia Talarico Saia
• Support Opportunities: Program for Research on Bioenergy (BIOEN) - Regular Program Grants