气相色谱-三重四极杆质谱法测定人体血清中新型溴代阻燃剂  

Determination of novel brominated flame retardants in human serum by gas chromatography-triple quadrupole mass spectrometry

作　　者：刘美 张高信 张晓莉 孙丽鹏 杨晓春 李英明[1] 张庆华[1,2,3] LIU Mei;ZHANG Gaoxin;ZHANG Xiaoli;SUN Lipeng;YANG Xiaochun;LI Yingming;ZHANG Qinghua(State Key Laboratory of Environmental Chemistry and Ecotoxicology,Research Center for Eco-Environmental Sciences,Chinese Academy of Sciences,Beijing,100085,China;College of Resources and Environment,University of Chinese Academy of Sciences,Beijing,100049,China;School of Environment,Hangzhou Institute for Advanced Study,University of Chinese Academy of Sciences,Hangzhou,310000,China;College of Chemistry and Chemical Engineering,Northwest Normal University,Lanzhou,730070,China;Shimadzu(China)Co.,Ltd.Innovation Center,Beijing,100020,China)

机构地区：[1]中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室,北京100085 [2]中国科学院大学资源与环境学院,北京100049 [3]国科大杭州高等研究院环境学院,杭州310000 [4]西北师范大学化学化工学院,兰州730070 [5]岛津企业管理(中国)有限公司创新中心,北京100020

出　　处：《环境化学》2023年第5期1502-1508,共7页Environmental Chemistry

基　　金：国家重点研发计划(2017YFC1600301);国家自然科学基金(22076215);中国科学院生态环境研究中心-岛津企业管理(中国)有限公司环境污染物仪器分析创新研发项目资助.

摘　　要：新型溴代阻燃剂(NBFRs)作为多溴二苯醚(PBDEs)的替代品,具有优良的防火性能.但有研究发现,NBFRs可能存在神经毒性和发育毒性等作用,从而对人体造成潜在的健康风险.血清作为人体内暴露的重要生物标志物,对评估健康风险具有重要意义.目前关于人体血清中NBFRs的健康风险研究较少,且血清中NBFRs含量低,前处理程序繁琐,基质复杂,给NBFRs的分析检测带来了很大困难.本研究建立并优化了人体血清中五溴苯(PBBz)、五溴甲苯(PBT)及十溴二苯基乙烷(DBDPE)等9种NBFRs的前处理,及气相色谱-三重四极杆质谱检测方法.血清样品经乙酸乙酯提取后,再经HLB固相萃取柱和弗罗里土-硅胶复合柱净化.采用电子轰击离子源(EI)和多反应监测(MRM)模式进行仪器分析.实验结果表明,血清样品中9种NBFRs的平均加标回收率在74%—136%之间,相对标准偏差小于21%.实际血清样品测试发现,内标物的回收率稳定在72%—126%之间,具有良好的检测效果.该方法前处理流程简单、稳定性好、灵敏度高,能广泛用于人体血清中NBFRs的分析.Novel brominated flame retardants(NBFRs)are considered as the commercial replacements for polybrominated diphenyl ethers(PBDEs).The potential neurotoxicity and developmental toxicity of NBFRs could cause adversely effects to human health.Serum is regarded as an important biomarker for human exposure,which presented great significance in assessing human health risks.Few studies reported the health risks of NBFRs in human serum.The analysis and detection of NBFRs were limited by the low concentration,complicated pretreatment processes and matrix effect.In this study,gas chromatography-triple quadrupole mass spectrometry(GCMS/MS)was established and optimized to detected the 9 NBFRs,mainly including pentabromobenzene(PBBz),pentabromotoluene(PBT)and decabromodiphenylethane(DBDPE).Serum samples were extracted by ethyl acetate,then cleaned up with HLB solid phase extraction column and Florisil-silica composite column.Electron impact(EI)ion source and multiple reaction monitoring(MRM)mode were applied for instrumental analysis.The average recoveries of the 9 NBFRs in serum samples were between 74%and 136%,and the relative standard deviation was less than 21%.Actual serum samples were collected to detect the 9 NBFRs,and the average recoveries of the internal standards ranged from 72%to 126%,which showed satisfactory performance.The developed methodology presented simple procedures,excellent stability and notable sensitivity,which was an efficient approach for the analysis of NBFRs in human serum.

关 键 词：新型溴代阻燃剂 人体血清 气相色谱-三重四极杆质谱 

分 类 号：R114[医药卫生—卫生毒理学] O657.63[医药卫生—公共卫生与预防医学]