Simultaneous Determination of Pyrethroid Insecticides in Foods of Animal Origins Using the Modified QuEChERS Method and Gas Chromatography-Mass Spectrometry

Abstract

Pyrethroid insecticides are used in agriculture to treat parasites in livestock. This study developed a simultaneous residue analysis method to measure seventeen pyrethroid insecticides in foods of animal origin, including beef, pork, chicken, milk, and eggs. The method, which comprises instrumental analysis using gas chromatography-tandem mass spectrometry and a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method for pretreatment, was optimized to verify the applicability of the method. A mixture of acetonitrile, ethyl acetate, and original salt (MgSO4 4 g, NaCl 1 g) was used as the extraction solvent and salt. MgSO4 (150 mg) primary secondary amine (25 mg) and graphitized carbon black (25 mg) were selected for dispersive solid phase extraction (d-SPE). The method limit of quantitation was 0.01 mg/L, and the linearity of the matrix-matched calibration curves was reasonable (R2 > 0.99). Recovery tests were performed at three concentrations (LOQ, 10 LOQ, and 50 LOQ). Good recoveries (75.2109.8%) and reproducibility (coefficient of variation <10%) were obtained. The matrix effects were in the range of –35.8 to 56.0%. The established method was fully validated and can be used as an official analytical method for quantifying pyrethroid insecticides in animal commodities.