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用超临界 1,1,1,2-四氟乙烷(R134a)从房屋灰尘中萃取多溴二苯醚(PBDEs)

Supercritical fluid extraction of polybrominated diphenyl ethers (PBDEs) from house dust with supercritical 1,1,1,2-tetrafluoroethane (R134a).

机构信息

Villanova University, Department of Chemistry, 800 Lancaster Avenue, Villanova, PA 19085, USA.

出版信息

Talanta. 2010 Jan 15;80(3):1116-20. doi: 10.1016/j.talanta.2009.08.038.

Abstract

The extraction of polybrominated diphenyl ethers (PBDEs) from SRM 2585 (Organic Contaminants in House Dust) was investigated using supercritical fluid R134a as an extraction solvent. Three methods of dust extraction were studied: (1) extraction of dry dust, (2) extraction of dry dust dispersed on Ottawa sand and (3) extraction of dust wet with dichloromethane. For each of the three sample preparation methods, extracts at three temperatures (110, 150, and 200 degrees C) above the critical temperature of R134a were performed. Eight PBDE congeners (BDE-28, -47, -99, 100, -153, -154, -183, and -209) in the SFE extracts were analyzed by liquid chromatography negative-ion atmospheric pressure photoionization tandem mass spectrometry (LC/NI-APPI/MS/MS). The optimum extraction of PBDEs from house dust using supercritical R134a is obtained when the dust is pre-wet with dichloromethane prior to extraction to swell the dust. For all sample preparation methods, higher temperatures afforded higher percent recoveries of the eight PBDE congeners. Only a combination of high-temperature (200 degrees C) and pre-wetting the dust with dichloromethane produced high recovery of the environmentally important, fully brominated PBDE congener, BDE-209.

摘要

采用超临界流体 R134a 作为萃取溶剂,从标准参考物质 2585(房屋灰尘中的有机污染物)中提取多溴二苯醚(PBDEs)。研究了三种灰尘提取方法:(1)干燥灰尘的提取,(2)在渥太华砂上分散的干燥灰尘的提取,以及(3)用二氯甲烷润湿的灰尘的提取。对于这三种样品制备方法中的每一种,都在超临界 R134a 的温度(110、150 和 200 摄氏度)以上进行了三个温度下的萃取。使用液相色谱负离子大气压光电离串联质谱法(LC/NI-APPI/MS/MS)分析了 SFE 提取物中的八种 PBDE 同系物(BDE-28、-47、-99、100、-153、-154、-183 和 -209)。使用超临界 R134a 从房屋灰尘中最佳提取 PBDE 的方法是在提取前先用二氯甲烷预先润湿灰尘,以使灰尘膨胀。对于所有样品制备方法,较高的温度会提高八种 PBDE 同系物的回收率。只有高温(200 摄氏度)和用二氯甲烷预先润湿灰尘的组合才能产生高回收率的环境重要的完全溴化 PBDE 同系物 BDE-209。

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