海产品中九种多溴联苯醚残留的气相色谱-负化学离子源/质谱法分析

Analysis of Nine Polybrominated Diphenyl Ethers Residue in Marine Samples by Gas Chromatography-Negative Chemical Ionization/Mass Spectrometry

建立了海产品中九种多溴联苯醚（PBDEs）残留的气相色谱-负化学离子源／质谱（GC-NCI／MS）分析方法。采用正己烷提取剂超声提取、Florisil硅藻土净化柱净化和正己烷洗脱剂洗脱的样品前处理方法，以PCB-103作为内标物，以GC-NCI／MS的选择离子监测方式（SIM）对海产品中九种PBDEs残留进行了定性与定量分析。分析方法的线性相关系数均≥0．9988，九种PBDEs两种添加浓度水平时的平均加标回收率为88．1％～97．3％，相对标准偏差为2．0％～6．6％，方法检出限均小于0．106ng／g。线性范围除PBDE-183为0．60～300．0ng／g外，其余八种PBDEs为0．50～250．0ng／g。同时分析了紫菜、海带、鲜海带、鱼干和花蛤干等海产品，在这些海产品干货中都检出了较多种的PBDEs残留。

In this paper, gas chromatography coupled with negative chemical ionization mass spectrometric （GC-NCI/MS） was described to detect the residue of nine polybrominated diphenyl ethers in marine samples. Samples was extracted by hexane and cleaned up on a Florisil column, then were determined by GC-NCI/MS in the selected ion monitoring mode and with PCB-103 as the internal standard. The recovery studies were performed at 10. 0 and 25. 0 ng/g fortification levels for eight PBDEs（12. 0 and 30. 0 ng/g for PBDE-183）, and the recoveries ranged from 88.1%-97.3% with a relative standard deviation between 2.0%-6.6%. The developed method was linear over the range of 0.50-250. 0 μg/L （for PBDE 183. 0. 60-300. 0 μg/L） with correlation coefficient in the range of 0. 9988-0. 9999, and the detection limits are lower than 0. 106 ng/g. The method was successfully applied to the determination of nine polybrominated diphenyl ethers residue in five marine samples.