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联用液相色谱/电子顺磁共振光谱法/电喷雾电离质谱法进行自由基鉴定

Combined liquid chromatography/electron paramagnetic resonance spectrometry/electrospray ionization mass spectrometry for radical identification.

作者信息

Iwahashi H, Parker C E, Mason R P, Tomer K B

机构信息

Laboratory of Molecular Biophysics, National Institute of Environmental Health Sciences, Research Triangle Park, North Carolina 27709.

出版信息

Anal Chem. 1992 Oct 1;64(19):2244-52. doi: 10.1021/ac00043a011.

Abstract

Electron paramagnetic resonance (EPR) spectrometry and mass spectrometry (MS) have been coupled together on-line with liquid chromatography (LC)/UV detection. These combined techniques have been applied to the determination of spin-trapped radical adducts, including phenyl, 2-, 3-, and 4-chlorophenyl, and 2-bromophenyl radicals trapped with alpha-(1-oxo-4-pyridyl)-N-tert-butylnitrone (4-POBN), and phenyl radicals trapped with 2-methyl-2-nitrosopropane (MNP), alpha-phenyl-N-tert-butylnitrone (PBN), and 5,5-dimethyl-1-pyrroline N-oxide (DMPO). Oxidized and reduced forms of the radical adducts were also detected by the on-line LC/EPR/MS system.

摘要

电子顺磁共振(EPR)光谱法和质谱法(MS)已与液相色谱(LC)/紫外检测在线联用。这些联用技术已应用于自旋捕获自由基加合物的测定,包括用α-(1-氧代-4-吡啶基)-N-叔丁基硝酮(4-POBN)捕获的苯基、2-、3-和4-氯苯基以及2-溴苯基自由基,以及用2-甲基-2-亚硝基丙烷(MNP)、α-苯基-N-叔丁基硝酮(PBN)和5,5-二甲基-1-吡咯啉N-氧化物(DMPO)捕获的苯基自由基。在线LC/EPR/MS系统还检测到了自由基加合物的氧化态和还原态。

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