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Development of dispersive liquid-liquid microextraction coupled with capillary liquid chromatography for determination of fipronil and its two metabolites
Jirková, Tereza ; Nováková, Lucie (advisor) ; Horstkotte, Burkhard (referee)
1 ABSTRACT Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Tereza Jirková Supervisors: Dr. Francisco J. Lara prof. PharmDr. Lucie Nováková, Ph.D Title: Development of dispersive liquid-liquid microextraction coupled with capillary liquid chromatography for determination of fipronil and its two metabolites Fipronil is a phenylpyrazolic insecticide that is prohibited for use in food-producing animals. This diploma thesis proposes a green analytical methodology for the study of residual fipronil and its two degradation products, fipronil sulfone and fipronil sulfide. For their determination, a method of capillary liquid chromatography with UV detection was developed and validated. Correlation coefficients above 0.998 confirm good linearity and the study of repeatability with values not exceeding 2.9% RSD shows high precision of this method. For the dispersive liquid-liquid microextraction method used for sample preparation, the dispersing and extracting solvents were optimized. The results show that the highest recoveries 82% - 92% were achieved with dibromomethane as an extractant and acetonitrile as a dispersant. All the experiments were carried out with standard solutions and in further studies this methodology should be transferred to egg or other...

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