Method Development and Validation for the Determination of Fipronil and Its Metabolite Residues in Eggs and Products
Keywords:
Fipronil, Eggs, GC-MS/MS, QuEChERS, MonitoringAbstract
Fipronil is an insecticide whose degradation products are highly neurotoxic for humans. In Thailand, fipronil is approved to use for plant protection but not as a veterinary drug. It was found that, egg contamination by fipronil in Europe in 2017 has generated concerns in Thai consumers. Thus, an analytical method is required for the investigation of the fipronil residues in commercialized egg and egg products in Thailand. Fipronil was extracted by a developed procedure based on EN 15662:2018 QuEChERS, detected by selected reaction monitoring techniques in GC-MS/MS and quantified by matrix-matched calibration curve. The validation of the method to detect fipronil and two metabolites, fipronil-desulfinyl, and fipronil-sulfone, in chicken and duck eggs showed that the LOD and the LOQ were 0.002 and 0.005 mg/kg, respectively. Satisfactory recoveries were obtained in the range of 92.9–111.6% in spiked samples at 0.005, 0.05 and 0.1 mg/kg with RSD lower than 8.6%. The relative standard uncertainty value was less than 20% and the method working ranges were between 0.005–0.5 mg/kg which were acceptable. This method was sensitive, precise, reliable, and suitable for use in the laboratory. The validated method was further applied for the analysis of 66 egg and egg product samples collected from Bangkok Metropolitan Region in 2021. The result showed no detectable fipronil residues in any samples. Overall results indicated that the described method would be applied for detecting the fipronil and its metabolite residues in the future.
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