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目的建立小龙虾中五氯酚的气相色谱测定方法。方法小龙虾中的五氯酚用正己烷在酸性条件下提取后用碳酸钾反萃取,加入乙酸酐衍生化为五氯酚苯乙酸酯,用HP-5非极性毛细管色谱柱分离后,用气相色谱法(电子捕获检测器)测定五氯酚的含量。结果五氯酚在0～400μg/L浓度范围内线性关系良好,相关系数为0.999 86。方法用于小龙虾分析,回收率在71.3%～88.4%之间,测定值的相对标准偏差(RSD)为1.08%。结论该方法操作简易、精密度高、回收率良好。
Objective To establish a method for the determination of pentachlorophenol in crayfish by gas chromatography. METHODS: Pentachlorophene in crayfish was extracted with n-hexane under acidic conditions and then back extracted with potassium carbonate. Acetic anhydride was derivatized to pentachlorophenol phenylacetate and separated by HP-5 apolar capillary column. The content of pentachlorophenol was determined by gas chromatography (electron capture detector). Results The linearity of pentachlorophenol in the range of 0 ~ 400μg / L was good with a correlation coefficient of 0.999 86. The method was applied to the analysis of crayfish with the recoveries between 71.3% and 88.4%. The relative standard deviation (RSD) of the measured values was 1.08%. Conclusion The method is simple, high precision and good recovery.