Multiresidue determination of polybrominated biphenyls (PBBs) and polybrominated diphenyl ethers (PBDEs) in egg samples by gas chromatography-mass spectrometry
建立了气相色谱-负离子化学源-质谱法(gC-nCI-MS)同时分析禽蛋食品中10种多溴联苯(PbbS)和多溴联苯醚(PbdES)残留的分析方法。禽蛋食品用正己烷超声提取、浓硫酸酸化、中性和酸性硅胶层析柱净化和正己烷洗脱后,以PCb209为内标物,采用gC-nCI-MS的选择离子监测方式(SIM)分析;同时探讨了目标物PbdE100 nCI-MS特征离子的断裂机理。当禽蛋食品空白的加标质量浓度为5(3.5)和50(35)μg/kg时,加标回收率为75.2%~107%,相对标准偏差为2.3%~8.8%,方法检测限为0.14~0.39μg/kg,线性范围为1~250μg/kg,相关系数皆大于0.9991,方法已用于禽蛋食品中10种痕量PPbS和PbdES残留的同时分析。A method for the simultaneous determination of 10 PBBs and PBDEs in egg samples was developed.PBBs and PBDEs were extracted from egg samples with hexane and cleaned up on an acid silica gel column,then were determined by using gas chromatography-mass spectrometry operated in negative chemical ionization mode and quantified in selective ion monitoring mode,and with PCB209 as internal standard.Meanwhile,fragmentation mechanism of PBDE100 negative chemical ionization mass spectrometry was evaluated.Recovery studies were performed at 5(3.5) and 50(35) μg/kg fortification levels for each PBDEs(PBBs),and the recoveries ranged from 75.2% to 107% with relative standard deviations between 2.3% and 8.8% for the different PBDEs and PBBs.The developed method was linear over the range of 1～250 μg/kg,with correlation coefficients more than 0.9991.Finally,the developed analytical method has been applied to the determination of PBDEs and PBBs in several egg samples.国家基础科学人才培养基金(J0630429)项目资
