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    题名: Combining microwave-assisted extraction and liquid chromatography-ion-trap mass spectrometry for the analysis of hexabromocyclododecane diastereoisomers in marine sediments
    作者: Wu,HH;Chen,HC;Ding,WH
    贡献者: 中央大學
    关键词: POLYBROMINATED DIPHENYL ETHERS;BROMINATED FLAME RETARDANTS;SOIL;PESTICIDES;DUST;AIR
    日期: 2009
    上传时间: 2010-06-29 19:45:02 (UTC+8)
    出版者: 化學研究所
    摘要: An efficient microwave-assisted extraction (MAE) procedure coupled with high performance liquid chromatography-electrospray-ion-trap mass spectrometry (HPLC-ESI-ITMS) has been evaluated to determine hexabromocyclododecane diastereoisomers (alpha-, beta- and gamma-HBCD) in marine sediments. The composition of the LC mobile phase (consisting of water, methanol and acetonitrile) and the parameters of electrospray ionization (ESI) were evaluated to obtain chromatographic baseline separation and high sensitivity for the detection of these diastereoisomers. The effects of various operating parameters on the quantitative extraction of the HBCDs through MAE were systematically investigated. The three diastereoisomers were then quantitated by HPLC-ITMS employing ESI operated in the negative ionization mode. The HBCDs were extracted from the sediments through MAE using 40 mL of acetone/n-hexane (1/3, v/v) at 90 degrees C for 12 min. The limits of quantitation (LOQ) ranged from 25 to 40 pg/g (dry weight) in 5 g of the sediment samples. The recoveries of the HBCDs in spiked sediment samples ranged from 68 to 91% (relative standard derivation: 2-11%). The extraction efficiency of the MAE technique was also compared with Soxhlet extraction and pressurized liquid extraction. (C) 2009 Elsevier B.V. All rights reserved.
    關聯: JOURNAL OF CHROMATOGRAPHY A
    显示于类别:[化學研究所] 期刊論文

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