QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of 21 Succinate Dehydrogenase Inhibitor Fungicides in Animal Foods
By optimizing the conditions of QuEChERS salt-out extraction and dispersive solid-phase extraction,a method for the determination of 21 kinds of succinate dehydrogenase inhibitor(SDHI)fungicide residues in animal-derived foods(livestock and poultry products,aquatic products,viscera,fat,milk and egg)was established based on high performance liquid chromatography-triple quadrupole tandem mass spectrometer(HPLC-MS/MS).Based on the characteristics of different types of animal-derived food substrates,the extraction solvent,dehydrator and purification agent were optimized with the recovery and purification efficiency as the criteria to achieve efficient extraction of target substances and effective removal of matrix impurities.At the same time,better chromatographic columns and mobile phases were selected to improve the sensitivity and separation efficiency of target analytes.The samples were evenly dispersed with water,extracted with acetonitrile saturated with n-hexane,and cleaned up with PSA and C18 adsorbents.The extracts were separated on Thermo Accucore aQ column(150 × 2.1 mm,2.6 μm)using 5 mmol/L ammonium formate,0.1％ formic acid aqueous solution and methanol solution as mobile phase by gradient elution.The detection of SDHIs was detected by HPLC-MS/MS with positive electrospray ion source under multiple reaction monitoring(MRM)mode.The matrix-matched external standard method was used for the quantitation.The method showed good linearities in the range of 1-50 μg/L.The correlation coefficients(r)were greater than 0.999.The limits of detection(LODs)were in the range of 0.005-0.28 μg/kg.The limits of quantitation(LOQs)were in the range of 0.02-0.93 μg/kg.The standard solution was added to the blank sample matrix of pork,fat,milk and egg of different categories of animal origin.The average recoveries obtained ranged from 83.0％ to 107％ and the relative standard deviations(RSDs)from0.20％to 7.40％for spiking levels of 5,10 and 50 μg/kg.The proposed method was applied successfully for the residue determination of the selected pesticides in animal foods.
Animal-derived foodsSuccinate dehydrogenaseDispersive solid-phase extractionHigh performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)
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