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| Determination of Four Kinds of Novel Brominated Flame Retardants in Sediments by Gas Chromatography-Mass Spectrometry Combined with Accelerated Solvent Extraction-Synchronous Purification |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:accelerated solvent extraction（ASE） solid phase extraction（SPE） gas chromatography-mass spectrometry（GC-MS） sediments brominated flame retardants |
| Author | Institution |
| PEI Jing-cheng,WU Ming-hong,XIANG Jia-jia,PENG Bing-quan,XU Gang,SUN Yan-feng,GU Jian-zhong,LEI Jian-qiu |
1.上海大学环境与化学工程学院;2.中国科学院上海光学精密机械研究所 |
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| Abstract: |
| A simple method based on accelerated solvent extraction（ASE） /solid phase extraction（SPE） coupled with gas chromatography-mass spectrometry（GC-MS） was developed for the simultaneous determination of 2-ethylhexyl-2,3,4,5-tetrabromobenzoate（TBB）,1,2-bis（2,4,6-tribromophenoxy） ethane（BTBPE）,bis（2-ethylhexyl） 2,3,4,5-tetrabromophthalate（TBPH） and decabromodiphenylethane（DBDPE） in sediments.Extraction and cleanup of four novel brominated flame retardants in lyophilized sediments were performed by improved accelerated solvent extraction（ASE）,and the concentrated solution was cleanup using Florisil solid phase extraction cartridges with 4 mL hexane,then eluted with 4 mL dichloromethane.The eluents was concentrated under a gentle N2 stream and analyzed by GC-MS.The calibration curves were linear in the range of 20-10 000 μg?L-1 for DBDPE,and 2-1.000 μg?L-1 for the rest of compounds，with correlation coefficients more than 0.995.The instrumental limits of quantitation（S/N≥10） for target compounds were in the range of 0.074-44.4 μg?kg-1.The average recoveries of target compounds at two spiked levels（2,10 μg?L-1） were in the range of 79.5%-119.7%,with relative standard deviations（RSDs） of 2.6%-15.3%.The proposed method was applied in the determination of four novel brominated flame retardants in sediments at six different sediments sampling sites from principal watersheds of Shanghai.All samples were detected to be contain TBB,BTBPE,TBPH and DBDPE,except one sampling site without TBB.The method was simple and sensitive,and could meet the requirements for rapid and accurate determination of four novel brominated flame retardants． |
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