Abstract: GC was applied to the determination of sodium pentachlorophenol in environment media, i.e. sediment, carex cinerascens and water of Poyang lake wetland. After acidification, the sample was extracted with n-hexane and then reextracted with potassium carbonate solution. The derivatization was adopted with acetic anhydride and then the derivative was extracted with n-hexane. The quantitative and qualitative analysis were used by GC and GC-MS respectively. The analyte was separated on WondaCAP 1 chromatographic column (30 m×0.32 mm, 0.25 μm) and detected by ECD in GC determination. Linear relationship between values of peak area and mass concentration of sodium pentachlorophenol was kept in the range of 50.0-2 000 ng·L^-1, with detection limit (3S/N) of 15.0 ng·L^-1. Values of recovery found by standard addition method were in the range of 94.1%-106%, and values of RSDs (n=5) were in the range of 0.50%-2.2%.