摘要
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.
出处
《分析试验室》
CAS
CSCD
北大核心
2008年第7期30-34,共5页
Chinese Journal of Analysis Laboratory
基金
国家基础科学人才培养基金(J0630429)项目资助
关键词
GC—NCI/MS
动物肝脏
多溴联苯醚
溴系阻燃剂
Gas chromatography-negative chemical ionization/mass spectrometry
Animal liver
Polybrominated diphe- nyl ethers
Brominated flame retardants