首页> 外文期刊>Journal of Chromatographic Science >Determination of Pentachlorophenol Residue in Meat and Fish by Gas Chromatography-Electron Capture Detection and Gas Chromatography-Mass Spectrometry with Accelerated Solvent Extraction
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Determination of Pentachlorophenol Residue in Meat and Fish by Gas Chromatography-Electron Capture Detection and Gas Chromatography-Mass Spectrometry with Accelerated Solvent Extraction

机译:气相色谱-电子捕获检测和气相色谱-质谱联用加速溶剂萃取法测定肉和鱼中五氯苯酚残留

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摘要

A novel analytical method, using gas chromatography-electron capture detection (GC-ECD) and GC-mass spectrometry detection (MS), was developed for the qualitative and quantitative measurement of pentachlorophenol in meat and fish. The analyte was extracted by methanol-2% trichloroacetic acid (3/1, v/v) with accelerated solvent extraction (ASE). The eluted fraction was evaporated and derivatized with acetic anhydride-pyridine (1/1, v/v) for GC-ECD analysis and GC-MS confirmation. The parameters for extraction pressure, temperature and cycle of ASE, cleanup, derivatization and analysis procedure were optimized. The averaged decision limits and detection capability of the method were in the ranges of 0.25-0.41 and 0.49-1.01 (μg/kg in the muscle and liver of swine and bovine and in the muscle of carp and finless eel, respectively. Spiked recoveries from levels of 0.5-2.0 μg/kg were found to be more than 71.1%, with relative standard deviation less than 14.7% in GC-ECD and GC-MS. This rapid and reliable method can be used for the characterization and quantification of residues of pentachlorophenol in animal and fish tissues.
机译:建立了一种气相色谱-电子捕获检测(GC-ECD)和气相色谱-质谱检测(MS)的新型分析方法,用于肉和鱼中五氯苯酚的定性和定量测量。用加速溶剂萃取(ASE)的2%甲醇/三氯甲醇(3/1,v / v)萃取分析物。蒸发洗脱的级分,并用乙酸酐-吡啶(1/1,v / v)衍生化,用于GC-ECD分析和GC-MS确认。优化了萃取压力,ASE的温度和循环,纯化,衍生化和分析程序的参数。该方法的平均判定限和检测能力在0.25-0.41和0.49-1.01(μg/ kg,分别在猪和牛的肌肉和肝脏以及鲤鱼和无鳍鳗的肌肉中)之间。在GC-ECD和GC-MS中,0.5-2.0μg/ kg的含量大于71.1%,相对标准偏差小于14.7%,该快速可靠的方法可用于残留物的表征和定量。动物和鱼类组织中的五氯酚。

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