目的:建立鱼体中微量五氯酚及其盐类残留的毛细管气相色谱测定法。方法:样品加碳酸钾溶液使待测组分转化成可溶性盐,过滤,滤液经硫酸酸化后用正己烷提取,再加入乙酸酐衍生化生成五氯苯乙酸酯,经毛细管柱分离后用电子捕获检测器检测,峰高定量。结果:方法线性范围为0.01 mg/kg～50 mg/kg,最低检出限为1.0μg/kg,,加标回收率和相对标准差分别为76.2%～82.1%和14.5%。结论:该方法操作简单,灵敏度高,可用于鱼体中五氯酚钠残留测定。 Objective: To establish a method for the determination of trace pentachlorophenol and its salts in fish by capillary gas chromatography. Methods: The sample was added with potassium carbonate solution to convert the analyte into soluble salt, which was filtered. The filtrate was acidified with sulfuric acid and extracted with n-hexane. Acetic anhydride was derivatized to give pentachlorophenylacetate. After separation by capillary column, Capture detector detection, peak height quantitative. Results: The linear range of the method was 0.01 mg / kg ~ 50 mg / kg. The minimum detectable limit was 1.0 μg / kg. The recoveries and relative standard deviations were 76.2% -82.1% and 14.5%, respectively. Conclusion: The method is simple, sensitive and can be used for the determination of sodium pentachlorophenol in fish.