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Determination of pentachlorophenol and sodium pentachlorophenolate in fishery products by acetic anhydride derivatization/GC/μ-ECD

机译:乙酸酐衍生化/ GC /μ-ECD测定渔业产品中五氯苯酚和五氯苯酚钠

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A method was estimated to detect pentachlorophenol and sodium pentachlorophenolate in fishery products by gas chromatography with μ-ECD detector. Procedures of the method included extraction, alkaline stripping and derivatization. The pH of sample matrix was modified to 3-4 by nitric acid solution (nitric acid: water 1:1). Target compounds were extracted by hexane first and 0.2 mol/L potassium hydroxide solution was used as stripping reagent to isolate pentachlorophenol from hexane. Acetic anhydride was taken as derivatizing reagent to convert target compounds into nonpolar ester compounds according to acylation reaction. Derivatized compound was extracted by hexane for the analysis of GC. The limit of detection is 2μg/kg. The average recoveries ranged from 73.01 to 104.68% spiked at 2.0,4.0,10.0μg/kg. And the relative standard deviations ranged from1.5 to 8.3%. The method can be used for the determination of pentachlorophenol and sodium pentachlorophenolate in fishery products, and it provides an rapid and acute method for food safety determination.
机译:估计通过用μ-ECD检测器气相色谱法检测渔业产品中五氯苯酚和五氯苯酚钠。该方法的方法包括提取,碱性汽提和衍生化。通过硝酸溶液(硝酸:水1:1)改性样品基质的pH至3-4。己烷首先用己烷萃取靶化合物,用0.2mol / L氢氧化钾溶液用作溶出试剂以将五氯苯酚免于己烷。将乙酸酐作为衍生化试剂,以根据酰化反应将靶化合物转化为非极性酯化合物。通过己烷萃取衍生化合物,用于分析GC。检测限为2μg/ kg。平均回收率范围为73.01至104.68%,以2.0,4.0,10.0μg/ kg尖刺。并且相对标准偏差范围为1.5至8.3%。该方法可用于测定渔业产品中五氯苯酚和五氯苯酚钠,为食品安全测定提供了一种快速和急性的方法。

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