食品中多溴联苯醚残留的气相色谱-串联质谱分析方法研究  

Study on the Analysis of PBDEs Residues in Food by Gas Chromatography-Tandem Mass Spectrometry

作　　者：张莉莉[1] 彭淑女[2] 赵汝松[1] 林竹光[2] 

机构地区：[1]山东省分析测试中心山东省大型精密分析仪器应用技术重点实验室,山东济南250014 [2]厦门大学化学化工学院分析科学重点实验室,福建厦门361005

出　　处：《分析测试学报》2010年第6期603-607,共5页Journal of Instrumental Analysis

基　　金：国家基础科学人才培养基金资助项目(J0630429);山东省科技发展计划资助项目(2009GG20001021-9)

摘　　要：建立了食品中8种多溴联苯醚（PBDEs）残留的气相色谱-串联质谱分析方法,初步解析了PBDEs的电子轰击串联质谱（EI MS/MS）图,为各种目标物的准确定性分析提供依据。以BDE-28、BDE-47、BDE-66、BDE-85、BDE-99、BDE-100、BDE-153、BDE-154为研究对象,对EIMS/MS各分析参数进行了优化。用超声提取-酸性硅胶层析柱净化的前处理方法制备样品,当空白样品的加标水平为10.0、25.0μg/kg时,8种PBDEs的平均加标回收率为82%-112%,相对标准偏差为3.1%-15%,方法检出限均低于1.5μg/kg;8种PBDEs的线性范围为10.0-500μg/kg,相关系数均大于0.994 7。A gas chromatography-tandem mass spectrometric method was developed for the determination of polybrominated diphenyl ethers（PBDEs） residues,including BDE-28,BDE-47,BDE-66,BDE-85,BDE-99,BDE-100,BDE-153 and BDE-154 in food sample.The electron ionization mass spectrometry/mass spectrometry（EI MS/MS） spectra of PBDEs were analyzed.Experimental parameters influencing the behaviour of compounds in the mode of EI MS/MS were investigated and optimized.The sample was extracted with hexane-acetone by ultrasonic assisted extraction and cleaned-up with silica and acidic silica.Under the optimal conditions,the method detection limit（MDL） was lower than 1.5 μg/kg,the average recoveries of 8 PBDEs from spiked samples at two fortification levels of 10.0 and 25.0 μg/kg varied from 82% to 112% with relative standard deviations（RSDs） of 3.1%-15%.The calibration curves of all PBDEs showed good linearities in the range of 10.0-500 μg/kg with correlation coefficients more than 0.994 7.The result indicated that the proposed method had great potential in the analysis of PBDEs residues in food.

关 键 词：气相色谱-串联质谱 溴系阻燃剂 多溴联苯醚 食品 

分 类 号：O657.63[理学—分析化学] TQ314.248[理学—化学]