动物肝脏中九种多溴联苯醚残留量的GC-NCI／MS分析

Determination of nine polybrominated diphenyl ethers residues in animal liver by gas chromatography-negative chemical ionization/mass spectrometry

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 （GCNCI/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 0.07μg/kg, the range of linearity is from 0.1 to 500.0μg/kg for the other eight PBDEs except 0.12 to 600.0μg/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.