A rapid analytical method for the determination of pentachlorophenol (PCP) residual in paper materials with 2, 4, 6-trichlomphenol as the internal standard was developed. The paper material was extracted ultrasonically using ethanol in 30 minutes. The concentrated PCP extract was dissolved by 0.1 mol/L potassium carbonate solution, followed by derivation with acetic anhydride. The derivative was extract by n-hexane, and then analyzed in gas chromatography-mass spectrometry (GC/MS). The separation was performed on a HP-5MS column (30 m×0.25 mm, 0.25 m film thickness). The limits of detection (LOD) and limits of quantitation (LOQ) of PCP in the method were 0.02 mg/kg and 0.07 mg/kg by calculating the diluted standard mixture with the 0.5 g of sample matrix, and the recovery was 85.0%~98.1% with relative standard deviation (RSD) less than 6%. The study revealed that the method was suitable for the determination of residual pentachlomphenol in paper materials．