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Validation of a method for extraction of polycyclic aromatic hydrocarbons from sewage sludge and analysis by GC-MS

机译:污水污泥中多环芳烃的提取方法验证及GC-MS分析

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In the present study, the solid-liquid extraction with low temperature purification was validated for the determination of 16 polycyclic aromatic hydrocarbons from sewage sludge by gas chromatography-mass spectrometry. Recoveries ranged 70-114% for naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a] anthracene and chrysene, while the compounds benzo[b] fluoranthene, benzo [k] fluoranthene, benzo[a] pyrene, indeno[1,2,3-cd] pyrene, dibenzo [a, h] anthracene and benzo[g, h, i] perylene showed recoveries of between 40 and 70%. The relative standard deviation was less than 13% for all of the compounds. Negative matrix effect was observed on the 10 compounds with less retention time in the chromatographic analysis and positive matrix effect noticed on the others. The limits of quantification were from 2 to 20 mu g kg(-1), about 30 times less than the maximum residue limit allowed in sludge by the European Union. The validated method produced quantification of 11 PAHs in one sludge sample at concentrations ranging 20-2000 mu g kg(-1).
机译:在本研究中,验证了采用低温纯化的固液萃取方法,可通过气相色谱-质谱法测定污水污泥中的16种多环芳烃。萘,、,、芴,菲,蒽,荧蒽,pyr,苯并[a]蒽和an的回收率在70-114%之间,而苯并[b]荧蒽,苯并[k]荧蒽,苯并[b] ,、茚并[1,2,3-cd] ,、二苯并[a,h]蒽和苯并[g,h,i] ylene的回收率在40%至70%之间。所有化合物的相对标准偏差均小于13%。在色谱分析中,保留时间较短的10种化合物被发现具有负基质效应,而其他化合物则具有正基质效应。定量限为2至20微克kg(-1),比欧盟污泥中允许的最大残留限量低约30倍。经过验证的方法可对一种污泥样品中的11种PAHs进行定量,浓度范围为20-2000μg kg(-1)。

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