A new cleanup method of dioxins in sediment using large volume injection gas chromatography online coupled with liquid chromatography

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• 作者：Fengmei Tang^a ; ^b ; Yuwen Ni^a ; Haijun Zhang^a ; Yun Li^a ; Jing Jin^a ; Longxing Wang^a ; Jiping Chen^a ; ^{chenjp@dicp.ac.cn}
• 关键词：EPA ; environmental protection agency ; GC ; gas chromatography ; HPLC ; high performance liquid chromatography ; HRGC/HRMS ; high resolution gas chromatography/high resolution mass spectrometer ; I-TEF ; international-toxic equivalency factor ; I-TEQ ; internationa
• 刊名：Analytica Chimica Acta
• 出版年：2012
• 期刊代码：2_00032670
• 类别：ch
• 出版时间：4 June, 2012
• 卷：729
• 期：Complete
• 页码：73-79
• 文件大小：603 K

摘要

A new cleanup method was developed and validated for the determination of polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans (PCDD/Fs) in sediment. The sample extract was first treated with sulfuric acid and then cleaned up by a large volume injection gas chromatography online coupled with liquid chromatography (LVI-GC-LC) system. PCDD/Fs in the extract were separated by a GC column (DB-5), selected cut, cool trapped and transferred to a LC column (alumina). The fraction of PCDD/Fs eluted from the alumina column was collected and concentrated for the instrumental analysis. Under the optimized conditions, LVI-GC-LC method achieved the recoveries of 57-102%for 2,3,7,8-substituted PCDD/Fs, which met the requirements of US Environmental Protection Agency (EPA) Method 1613 and were better than those obtained using the conventional multistep column cleanup method. Meanwhile, compared with the conventional method, the limit of detection (LOD) values of 2,3,7,8-substituted PCDD/Fs cleaned up by LVI-GC-LC method were decreased due to the high-efficiency removal of interferents. These results suggested that the LVI-GC-LC cleanup method was a promising alternative to the multistep cleanup procedure for the determination of dioxins in environmental samples.