Abstract: A study mentioned by the title was developed for simultaneous monitoring of multiple types of anti-insect drugs (including tetraimidazoles, nitroimidazoles, triazines, carbamates and organic nitrogen pesticides) in poultry meat. The homogenized samples (2±0.01) g were taken, and 5 mL of water and 10 mL of extractant solutions, which consisted of 1 mL of acetic acid, 600 mL of acetonitrile and 400 mL of ethyl acetate, were added. The mixture was vortexed for 20 min. 0.5 g of anhydrous MgSO₄ was added and the mixture was centrifuged for 5 min. The supernatant (5 mL) was taken and blown to dryness at 40 ℃ by nitrogen, then vortexed for 1 min after adding 1 mL of solution (consisting of 1 mL of formic acid, 900 mL of deionized water, and 100 mL of acetonitrile) and purified by 20 mg of C₁₈ powder and 30 mg of N-propylethylenediamine (PSA) powder in a cleanup tube. The result solution was filtered through a 0.22 μm double-layer microfiltration membrane.The 24 anti-insect drugs in filtrate was separated on GISTC18-AQ chromatographic column (100 mm×2.1 mm, 1.9 μm) as the stationary phase, using the mixtures of acetonitrile and 0.1%(volume fraction) formic acid solution at different volume ratios as the mobile phase for gradient elution. Multiple reaction monitoring mode was adopted in mass spectrometry analysis, with the matrix-matched method for quantification. As shown by the results, linear relationships between the corresponding mass spectrometry peak areas and mass concentrations of 24 anti-insect drugs were found in definite ranges, with detection limits (3S/N) in the range of 0.01—0.40 μg·kg⁻¹. Test for recovery was made by the standard addition method, giving results in the range of 61.2%—113%, with RSDs (n=6) of the determined values not more than 15%. This method was used to analyze 30 actual samples, and hydroxy dimetridazole was detected in only one duck meat sample with detection amount of 1.46 μg·kg⁻¹. The results were consistent with those obtained by the standard methods described in Announcement No. 197-10-2019 of the Ministry of Agriculture and Rural Affairs and SN/T 4809—2017.