Study On UPLC-MS/MS Analysis Method Of Flusilazole,Fipronil And Fipronil's Three Metabolites Residues In Five Animal Origin Foods

Recently,due to the abuse of pesticides,the increasing use of pesticides and the lack of government supervision,pesticide residues in agricultural products are becoming more and more prominent.Pesticide residue has become one of the main factors which affect the safety of plant origin food.Pesticide is widely used in agricultural production,and it is an important technology to ensure grain yield and harvest,but large-scale use of pesticides not only lead to environmental pollution,but also the accumulation of pesticide residues in livestock products is also accumulated through the food chain,causing pollution to animal products,and ultimately harming human health.Food safety accidents occur frequently in recent years,it makes people pay more attention to the quality and safety of animal products.Therefore,it is of great significance to develop fast,reliable and sensitive technology of pesticide residue to ensure human health,providing strong technical support for China's import and export trade.Three metabolites were produced under the action of hydrolysis and photolysis,respectively are Fipronil desulnyl,Fipronil sulfone and Fipronil sulfide.In this paper,we use QuEChERS technique to detect the residue of flusilazole,fipronil and its three metabolites in five animal origin foods including chicken,milk,eggs,porkliver and pork by combining ultra-high performance liquid chromatography-tandem mass spectrometry and this method was applied to 420 real samples from 14 provinces.The results of study are as following.The sample was extracted with acetonitrile solution,low temperature treatment,d-SPE purificaion of MWNTs,F and C18,BEH C₁₈8 as analytical column,the acetonitrile solution is a gradient elution separation for the flow phase,the total analysis runs no more than ten minutes,the quantification of external standard method.The scanning mode of MRM,qualitative screening and quantitative analysis were conducted with ESI-.Fipronil and its three metabolites show good linear relationship with the range of 10-1000?g/kg,r²?0.9901.Flusilazole show good linear relationship with the range of10-2000?g/kg,r²?0.9937.At different concentrations,the average recovery of fipronil and its metabolites in five animal origin foods is 72.1%-113.8%,RSD is 1.9-17.1%,LOD is 0.73-1.94?g/kg,LOQ is 10-200?g/kg.The average recovery of flusilazole in five animal origin foods is 79.6%-103.2%,RSD is 1.5-5.8%,LOD is0.62-1.75?g/kg,LOQ is 5-10?g/kg.The method is simple,sensitive and accurate.It is suitable for rapid screening and quantitative detection of flusilazole,fipronil and its metabolites in animal origin food and the sensitivity of the method meets the EU's residue limit requirements.The practical application of this method was applied to detect the residue of fipronil from 420animal origin foods in 14 provinces.None of these samples were detected with flusilazole and fipronil,indicating that none of these samples had flusilazole and fipronil residue.