河北省淡水鱼中五氯酚钠的残留调查
目的 建立淡水鱼组织中五氯酚钠的气相色谱-质谱测定方法, 并调查河北省市场上淡水鱼中五氯酚钠的污染状况。方法 鱼肉组织加入内标后, 经5%三氯乙酸沉淀, 液液萃取, SLC柱净化, 采用乙酸酐-吡啶溶液衍生成五氯苯氧乙酸酯, 气相色谱-质谱法测定, 内标法定量。结果 五氯酚在2.5～200 ng/mL范围内呈现良好的线性关系, r2=0.9990。方法检出限为0.15 μg/kg, 定量限为0.50 μg/kg。测得全省采集的66份淡水鱼样品中, 检出阳性样品3份, 检出范围2.82~6.22 μg/kg, 不合格率4.5%。结论 本方法灵敏、准确, 适用于鱼肉中五氯酚钠的定量测定, 能满足基层筛查要求。今后应重点加强水产品中五氯酚钠监测工作, 保障食品安全。
Objective To establish a method for the determination of sodium pentachlorophenol in freshwater fish tissues by gas chromatography-mass spectrometry (GC-MS), and to investigate the contamination of sodium pentachlorophenol in freshwater fish in Hebei province. Methods After adding internal standard, fish tissue was precipitated by 5% trichloroacetic acid, extracted by liquid-liquid, purified by SLC column, and then derived into pentachlorophenoxyacetate by acetic anhydride pyridine solution. The content was determined by GC-MS and quantified by internal standard method. Results The linear range of pentachlorophenol was 2.5?200 ng/mL, r2=0.9990. The limit of detection was 0.15 μg/kg and the limit of quantitation was 0.50 μg/kg. Among 66 freshwater fish samples collected in the whole province, 3 samples were positive, the detection range was 2.82?6.22 μg/kg, and the unqualified rate was 4.5%. Conclusion This method is sensitive, accurate and suitable for the quantitative determination of sodium pentachlorophenol in fish and can meet the requirements of primary screening. In the future, the monitoring of sodium pentachlorophenol in aquatic products should be strengthened to ensure food safety.
标题：河北省淡水鱼中五氯酚钠的残留调查
英文标题：Survey of sodium pentachlorophenate residues in freshwater fish of Hebei province
作者：
刘印平 河北省疾病预防控制中心
云鹏 河北省疾病预防控制中心
路杨 河北省疾病预防控制中心
王丽英 河北省疾病预防控制中心
陈福尊 河北省疾病预防控制中心
冯静 河北省疾病预防控制中心
董彬 河北省疾病预防控制中心
常凤启 河北省疾病预防控制中心
中文关键词:五氯酚钠,淡水鱼,污染调查,气相色谱-质谱法,河北省,
英文关键词:sodium pentachlorophenate,freshwater fish,pollution survey,gas chromatography-mass spectrometry,Hebei province,
发表日期：2020-05-09
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