Fast gas chromatography-atmospheric pressure (photo)ionization mass spectrometry of polybrominated diphenylether flame retardants
Fast gas chromatography-atmospheric pressure (photo)ionization mass spectrometry of polybrominated diphenylether flame retardants
复制标题
DOI：
10.1016/j.aca.2019.01.007
复制
发表时间：
2019-05-16
影响因子：
6.2
通讯作者：
Jobst, Karl J.
中科院分区：
文献类型：
--
作者：
Di Lorenzo, Robert A.;Lobodin, Vladislav V.;Jobst, Karl J.
气相色谱（GC）和质谱（MS）是分析环境毒物强有力的互补技术。目前，大多数气相色谱-质谱仪采用真空下的电子电离，但将气相色谱与大气压电离（API）耦合的概念正在引起人们的兴趣。API条件固有地与广泛的电离技术以及高载气流量兼容，从而实现快速GC分离。本研究报道了常压化学电离（APCI）和定制光电离（APPI）源在多溴联苯醚（PBDEs）的GC-MS分析中的应用，多溴联苯醚是一种普遍存在的阻燃剂。多溴二苯醚的光解离产生了大量的分子离子M中心点+，而碎片化很小。观察到一些光氧化反应，这区分了BDE的关键异构体。在GC-APPI中没有形成质子化分子[M+H](+)，因为H2O（簇）的电离能超过了电离光子的能量。避免混合模式电离是APPI相对于APCI的一个主要优点，后者需要仔细控制源条件。采用氦气和氮气载气建立了一种快速气相色谱- api -质谱联用方法，该方法可在7min （He）和15min （N-2）内分离临界异构体（BDE-49/71）和洗脱BDE- 209。结果表明，GC-APPI和GC-APCI方法与使用标准参考物质（NIST SRM 1944和SRM 2585）和选定的环境样品分析多溴二苯醚的既定方法的灵敏度相匹配，并提高了选择性和通量。(c) 2019年Elsevier B.V.出版
Gas chromatography (GC) and mass spectrometry (MS) are powerful, complementary techniques for the analysis of environmental toxicants. Currently, most GC-MS instruments employ electron ionization under vacuum, but the concept of coupling GC to atmospheric pressure ionization (API) is attracting revitalized interest. API conditions are inherently compatible with a wide range of ionization techniques as well high carrier gas flows that enable fast GC separations. This study reports on the application of atmospheric pressure chemical ionization (APCI) and a custom-built photoionization (APPI) source for the GC-MS analysis of polybrominated diphenyl ethers (PBDEs), a ubiquitous class of flame retardants. Photoionization of PBDEs resulted in the abundant formation of molecular ions M center dot + with very little fragmentation. Some photo-oxidation was observed, which differentiated critical BDE isomers. Formation of protonated molecules [M+H](+) did not occur in GC-APPI because the ionization energy of H2O (clusters) exceeds the energy of the ionizing photons. Avoiding mixed-mode ionization is a major advantage of APPI over APCI, which requires careful control of the source conditions. A fast GC-API-MS method was developed using helium and nitrogen carrier gases that provides good separation of critical isomers (BDE-49/71) and elution of BDE 209 in less than 7min (with He) and 15 min (with N-2). It will be shown that the GC-APPI and GC-APCI methods match the sensitivity and improve upon the selectivity and throughput of established methods for the analysis of PBDEs using standard reference materials (NIST SRM 1944 and SRM 2585) and selected environmental samples. (c) 2019 Published by Elsevier B.V.