Abstract: A residue analytical method was developed for the simultaneous determination of 13 pyrethroid pesticides in water-sediment system. Solid-phase extraction (SPE) and pressurized fluid extraction (PFE) were used as sample preparation method for water and sediment, respectively. Then gas chromatography-mass spectrometry (GC-MS) was used to detect the analytes in selective ion monitor (SIM) mode with internal standard method for quantification. The results showed that the linear relationship for the 13 pyrethroids was good with the correlation coefficient (R²) ≥ 0.995. The recoveries of the pyrethroids were 83%-104% and the relative standard deviation (RSD, n = 6) were 0.73%-6.8% at the spiking levels of 0.50-50 μg/L in water. The recoveries of the pyrethroids were 73%-92% and the RSD (n = 6) were 0.63%-5.3% at the spiking levels of 5.0-50 μg/kg in sediment. The detection limits were 1.0-7.0 μg/L, and the quantification limits were 0.50 μg/L and 5.0 μg/kg in water and sediment, respectively. The method is easy to operate with high sensitivity and reliable reproducibility, which is suitable for simultaneous determination of pyrethroid pesticides in water-sediment system.