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

Abstract

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.