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通过电子顺磁共振自旋捕集和质谱法在大鼠肝微粒体中检测到的卤代烃自由基代谢产物的结构。

The structure of free radical metabolites detected by EPR spin trapping and mass spectroscopy from halocarbons in rat liver microsomes.

作者信息

Sang H, Janzen E G, Poyer J L, McCay P B

机构信息

Free Radical Biology and Aging Research program, Oklahoma Medical Research Foundation, Oklahoma City 73104, USA.

出版信息

Free Radic Biol Med. 1997;22(5):843-52. doi: 10.1016/s0891-5849(96)00431-5.

DOI:10.1016/s0891-5849(96)00431-5
PMID:9119253
Abstract

Electron impact (EI) tandem mass spectrometry (MS/MS) combined with EPR spin trapping was used to detect and identify the free radical metabolites of various halocarbons in rat liver microsomal dispersions. EPR spectra of the spin adducts of radical metabolites derived from fluorine-containing halocarbons display fluorine hyperfine splitting, which can be used as proof for the identification of this kind of halocarbon-derived free radical spin adduct. For halocarbons without fluorine atoms, MS/MS was found to be a very useful and simple method for the detection and identification of the structures of halocarbon-derived spin adducts from radical metabolites. The molecular ions from spin adducts of these halocarbon-derived free radical intermediates were observed for the first time by scanning the precursor ion spectrum of m/z 57. These assignments were further confirmed by the use of perdeuterated tert-butyl PBN which provides the precursor ion spectrum of m/z 66.

摘要

电子轰击(EI)串联质谱(MS/MS)结合电子顺磁共振(EPR)自旋捕获技术,用于检测和鉴定大鼠肝微粒体分散液中各种卤代烃的自由基代谢产物。含氟卤代烃衍生的自由基代谢产物的自旋加合物的EPR谱显示氟超精细分裂,可作为鉴定这类卤代烃衍生的自由基自旋加合物的证据。对于不含氟原子的卤代烃,发现MS/MS是检测和鉴定自由基代谢产物中卤代烃衍生的自旋加合物结构的一种非常有用且简单的方法。通过扫描m/z 57的前体离子谱,首次观察到这些卤代烃衍生的自由基中间体的自旋加合物的分子离子。使用氘代叔丁基PBN提供m/z 66的前体离子谱,进一步证实了这些归属。

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