建立了动物肝脏中9种PBDEs残留量的气相色谱-负化学离子源/质谱(GC-NCI/MS)的分析方法。动物肝脏样品经V(正己烷)∶V(丙酮)=1∶1超声辅助提取,中性与酸性硅胶层析柱净化和V(正已烷)∶V(CH2Cl2)=1∶1洗脱和浓缩后,以PCB-103为内标物,采用GC-NCI/MS的选择离子监测方式(SIM)对其中的9种PBDEs残留量进行了定性与定量分析。当动物肝脏空白样品的加标质量浓度为5.0、20.0μg/kg(PBDE-183为6.0、24.0μg/kg)时,9种PBDEs的平均加标回收率为75.1%~88.2%,相对标准偏差为3.3%~7.9%,方法检出限均小于0.07μg/kg;线性范围除PBDE-183为0.12~600.0μg/kg外,其余8种PBDEs为0.1~500.0μg/kg,相关系数都大于0.9993。所建立的分析方法已用于5种动物肝脏的8个样品中9种PBDEs残留量的分析。An analytical method for the determination of nine polybrominated diphenyl ethers(PBDEs) residue in animal liver is described based on gas chromatography coupled with negative chemical ionization mass spectrometry(GC-NCI/MS).In this paper,hexane/acetone(1/1,V/V) and hexane/dichloromethane(1/1,V/V) were used as the extraction and elution solvents.After the extraction was cleaned by silica and acid silica,the analysis of nine PBDEs in samples was accomplished using GC-NCI/MS in the selected ion monitoring mode(SIM) with PCB-103 as the internal standard(IS).This method performs well: the average recoveries of spiked samples range from 75.1% to 88.2% with relative standard deviations between 3.3% and 7.9%,method detection limit is lower than 0.07 μg/kg,the range of linearity is from 0.1 to 500.0 μg/kg for the other eight PBDEs except 0.12 to 600.0 μg/kg for PBDE-183,with correlation coefficients larger than 0.9993.The method has been applied successfully to the determination of nine polybrominated diphenyl ethers residues in eight samples of five animal livers.国家基础科学人才培养基金(J0630429)项目资
