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大气压化学电离气相色谱-质谱法分析食品中选定的新型溴化阻燃剂。

Atmospheric Pressure Chemical Ionization Gas Chromatography Mass Spectrometry for the Analysis of Selected Emerging Brominated Flame Retardants in Foods.

机构信息

Beijing Advanced Innovation Center for Food Nutrition and Human Health, China Agricultural University, Beijing 100193, China.

College of Science, Beijing University of Chemical Technology, Beijing, 100029, China.

出版信息

Sci Rep. 2017 Mar 10;7:43998. doi: 10.1038/srep43998.

Abstract

Emerging brominated flame retardants (eBFRs) other than polybrominated diphenyl ethers (PBDEs), polybrominated biphenyls (PBBs) and their derivatives in foods have been in focus in recent years due to their increasing production volumes, indefinite information on toxicities and the lack of data on occurrence in environments, foods as well as humans. In this study, gas chromatography was coupled to an atmospheric pressure chemical ionization-tandem mass spectrometry (APGC-MS/MS) for the analysis of six eBFRs in pork, chicken, egg, milk and fish. A short section of unpacked capillary column coupled to the end of the analytical column was applied to improve the chromatographic behaviors of high boiling point compounds. The method was comprehensively validated with method limit of quantification (mLOQ) lower than 8 pg/g wet weight (w.w.). Samples from Chinese Total Diet study were quantified following the validated APGC-MS/MS method. 2,3,4,5-pentabromo-6-ethylbenzene (PBEB), hexabromobenzene (HBB), pentabromotoluene (PBT) and 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE) were most frequently detected in samples. The highest concentration was found in fish with 351.9 pg/g w.w. of PBT. This is the first report on the presence of PBT in food samples with non-ignorable concentrations and detection rate.

摘要

近年来,除多溴二苯醚(PBDEs)、多溴联苯(PBBs)及其衍生物外,食品中的新兴溴化阻燃剂(eBFRs)因其产量不断增加、毒性信息不确定以及环境、食品和人体中存在数据缺乏而受到关注。在这项研究中,采用气相色谱-大气压化学电离串联质谱(APGC-MS/MS)分析猪肉、鸡肉、鸡蛋、牛奶和鱼类中的 6 种 eBFRs。在分析柱的末端连接一段未填充的毛细管柱,以改善高沸点化合物的色谱行为。该方法通过定量下限(mLOQ)低于 8 pg/g 湿重(w.w.)进行了全面验证。采用经过验证的 APGC-MS/MS 方法对中国总膳食研究的样本进行定量分析。2,3,4,5-五溴-6-乙基苯(PBEB)、六溴苯(HBB)、五溴甲苯(PBT)和 1,2-双(2,4,6-三溴苯氧基)乙烷(BTBPE)是最常被检测到的物质。在鱼类样本中发现了最高浓度,其 PBT 浓度为 351.9 pg/g w.w.。这是首次报道食品样本中存在具有不可忽视浓度和检测率的 PBT。

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