气相色谱-质谱法同时测定河流沉积物中多环芳烃和有机氯农药
Simultaneous Determination of Polycyclic Aromatic Hydrocarbons and Organochlorine Pesticides in River Sediments by Gas Chromatography-Mass Spectrometry
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摘要: 建立了用加速溶剂萃取,气相色谱-质谱法同时测定河流沉积物中16种多环芳烃和19种有机氯农药的分析方法,优化了萃取溶剂、萃取温度和时间、凝胶渗透色谱收集时间、固相萃取洗脱溶剂和洗脱体积等条件。16种多环芳烃的方法检出限在0.15~0.59 ng/g,加标回收率为82%~102%,相对标准偏差(RSD, n=5)为1.1%~4.5%。19种有机氯农药的方法检出限在0.14~2.23 ng/g,加标回收率为71%~108%,相对标准偏差(RSD,n=5)为1.0%~4.5%。实际样品的测定结果表明,该方法分离效果较好,能够满足沉积物样品中多环芳烃和有机氯农药的分析要求。Abstract: A method for simultaneous determination of 16 polycyclic aromatic hydrocarbons (PAHs) and 19 organochlorine pesticides (OCPs) in river sediments by gas chromatography-mass spectrometry with accelerated solvent extraction (ASE) was established. The parameters of ASE, such as type of extraction solvent, extraction temperature and time, the collection time for gel permeation chromatograph, as well as the selection of elution agents and elution parameters in solid phase extraction (SPE) were optimized. The detection limits for 16 PAHs ranged from 0.15 to 0.59 ng/g (dry weight), and the recoveries for spiked samples were between 82% and 102% with precision of 1.1%~4.5% RSD (n=5). The detection limits for 19 OCPs ranged from 0.14~2.23 ng/g (dry weight), and the recoveries for spiked samples were between 71% and 108% with precision of 1.0%~4.5% RSD (n=5). The method has been applied to the determination of 16 PAHs and 19 OCPs in sediment samples with satisfactory results.
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