Combining microwave-assisted extraction and liquid chromatography-ion-trap mass spectrometry for the analysis of hexabromocyclododecane diastereoisomers in marine sediments
Combining microwave-assisted extraction and liquid chromatography-ion-trap mass spectrometry for the analysis of hexabromocyclododecane diastereoisomers in marine sediments
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DOI：
10.1016/j.chroma.2009.09.001
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发表时间：
2009-11-06
影响因子：
4.1
通讯作者：
Ding, Wang-Hsien
中科院分区：
文献类型：
--
作者：
Wu, Hsin-Hung;Chen, Hsin-Chang;Ding, Wang-Hsien
对高效微波辅助萃取程序与高效液相色谱-电喷雾-离子阱质谱联用（HPLC-ESI-ITMS）进行了评价，以测定海洋沉积物中的六溴环十二烷非对映异构体（α-、β-和γ-六溴环十二烷）。评价了LC移动的相组成（由水、甲醇和乙腈组成）和电喷雾电离（ESI）参数，以获得用于检测这些非对映异构体的色谱基线分离和高灵敏度。系统研究了各种操作参数对通过MAE定量提取六溴环十二烷的影响。然后通过HPLC-ITMS采用ESI以负离子化模式进行定量。使用40 mL丙酮/正己烷（1/3，v/v）在90 ℃下通过MAE从沉积物中提取六溴环十二烷12分钟。5 g沉积物样品的定量限（LOQ）范围为25至40 pg/g（干重）。六溴环十二烷在加标沉积物样品中的回收率为68%至91%（相对标准偏差：2-11%）。并与索氏提取法和加压液体提取法进行了比较。(C)2009 Elsevier B. V.保留所有权利。
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.