Journal
MICROCHEMICAL JOURNAL
Volume 178, Issue -, Pages -Publisher
ELSEVIER
DOI: 10.1016/j.microc.2022.107393
Keywords
Insecticide; Sample preparation; HPLC; Doehlert Matrix; Amazon turtle
Categories
Funding
- Financiadora de Estudos e Projetos [01.13.0371.00]
- Conselho Nacional de Desenvolvimento Cientifico e Tecnologico
- Coordenacao de Aperfeicoamento de Pessoal de Nivel Superior [001]
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The development and validation of a method for quantifying fipronil contamination in turtle eggshells is an urgent task. The proposed solid-liquid extraction with low-temperature partitioning method was optimized and successfully used to detect and quantify fipronil residues in amazon-turtle eggshell samples.
The intense use of fipronil in sugarcane crops in Brazil in regions close to the spawning areas of freshwater turtles may pose a considerable threat to the reproduction of these organisms. Therefore, the development and validation of a method to quantify the fipronil contamination in turtle eggshells is pressing and constitutes the main goal of the present study. The proposed method was based on solid-liquid extraction with low-temperature partitioning, reducing its scale due to the limited availability of turtle eggshell samples. The fipronil extraction from eggshell samples was optimized using a statistical design based on the Doehlert Matrix. Eggshell mass, the volume of extraction solvent, and the freezing time were the optimized method parameters, yielding fipronil recoveries close to 100% without a clean-up step. Furthermore, the optimized method was linear, robust, precise, and accurate in the fipronil concentration range of 8.4-1,818.0 mu g kg(-1). The limit of quantification for fipronil was 8.37 mu g kg(-1), about 2.5 times lower than the maximum residual limit for fipronil in eggs. Residues of fipronil were detected and quantified successfully in amazon-turtle eggshell samples using the proposed method. In conclusion, the one-step SLE-LTP method was mini-scaled for the first time and presented a strong potential for monitoring fipronil residues in freshwater turtle eggshells.
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