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0.106 ng/g。线性范围除PBDE-183为0.60~300.0 ng/g外,其余八种PBDEs为0.50~250.0 ng/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.国家基础科学人才培养基金(No.J0630429
