以2,4,6-三氯苯酚为内标，建立了纸质材料中五氯苯酚残留量的气相色谱/质谱联用（GC/MS）测定方法。0.5 g纸质材料样品以乙醇为萃取溶剂，超声提取30 min，提取液经浓缩后用碳酸钾水溶液溶解，经乙酸酐乙酰化后以正己烷提取，以HP-5MS色谱柱分离，采用选择离子扫描(SIM)方式对五氯苯酚进行了测定，内标法定量。实验结果表明，五氯苯酚线性关系良好(R2>0.9999)，在3种浓度（0.105 μg、0.315 μg和0.525 μg）的加标水平下，回收率为85.0%~98.1%，相对偏差小于6%，方法的检出限为0.02 mg/kg，定量限为0.07 mg/kg。方法的样品前处理过程简单，易操作，适用于纸质材料中五氯苯酚残留量的检测。

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．