微波萃取-气相色谱/质谱测定底泥中多溴联苯醚

Determination of Polybrominated Diphenyl Ethers in Sediments Using Microwave Extraction and GC-NCI-MS Spectrometry

文章建立微波萃取,复合硅胶氧化铝层析柱净化,气相色谱-负化学离子源质谱（GC-NCI-MS）检测对环境底泥样品中七种多溴联苯醚（PBDEs）单体定量分析的方法。底泥样品经25 mL正己烷：丙酮（1：1）萃取剂微波萃取10 min,过复合层析柱净化,70 mL正己烷：二氯甲烷（1：1）洗脱和浓缩后,加入内标物PCB-103后进行内标定量分析,7种PBDEs单体的平均基质加标回收率均值为88.6%96.7%,相对标准偏差为1.9%9.3%,方法检出限均小于0.06 ng/g,方法具有良好的重现性,较好的回收率和较高的灵敏度。所建立的分析方法体系已用于长江口近岸沉积物中7种PBDEs残留量的检测,四个实际样品中添加回收率指示物PCB-209,其回收率范围为79.5%109.6%,相对标准偏差为5.2%16.5%。

Method of determination of polybrominated diphenyl ethers（PBDEs）contained in sediments is developed,which involves microwave extraction,multilayer silica and alumina column for clean-up and GC-NCI-MS for final determination. According to the experimental result,average recoveries of spiked samples range from 88.6 to 96.7%,with relative standard deviations between 1.9%and 9.3%,detection limit of the method being less than 0.06 ng/g.Besides,it is reported that a system based on this method has been applied to a survey of aktological sediments in the Yangtze Estuary area,during which seven polybrominated diphenyl ethers are detected and measured.