Analysis of nitrated polycyclic aromatic hydrocarbons in diesel particulates

Analysis of nitrated polycyclic aromatic hydrocarbons in diesel particulates
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柴油颗粒物中硝化多环芳烃的分析

DOI:
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发表时间:
1982
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通讯作者:
D. Hunt
D. Hunt
中科院分区:
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文献类型:
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作者:
D. Schuetzle;T. Riley;T. Prater;T. M. Harvey;D. Hunt

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采用高效液相色谱、气相色谱/质谱、高分辨质谱和质谱/质谱(MS/MS)联用技术分析柴油机颗粒物提取物中的硝化多环芳烃(nitro-PAH)。采用三级四极杆串联质谱(TSQ/MS),在恒中性损失模式下,对柴油机微粒溶剂萃取物中的硝基多环芳烃异构体进行快速定性筛选。发现了20个这样的硝基PAH衍生物的异构体基团,其中许多基团含有大量可能的化合物。质量分析离子动能谱(MIKES)-MS/MS被发现是远低于TSQ-MS/MS的选择性分析的硝基多环芳烃的普通柴油抽提物。需要HPLC预分馏以去除MIKES分析中的干扰。熔融石英毛细管GC/MS使用柱上注射被认为是必要的识别特定的硝基PAH异构体和最大限度地减少分解。高度致突变的1-硝基芘(1-NP)是硝基(芘和荧蒽)异构体组中发现的唯一化合物。MIKES和TSQ技术对1-NP的定量结果相当。
The analysis of nitrated polycyclic aromatic hydrocarbons (nitro-PAH) in diesel particulate extracts using a combination of high-performance liquid chromatography, gas chromatography/mass spectrometry, high-resolution mass spectrometry, and mass spectrometry/mass spectrometry (MS/MS) techniques is described. Triple stage quadrupole (TSQ)-MS/MS operated in the constant neutral loss mode is described for the rapid qualitative screening of nitro-PAH isomer groups in solvent extracts of diesel particulates. Twenty such isomer groups of nitro-PAH derivatives were found, many of these groups containing a large number of possible compounds. Mass analyzed ion kinetic energy spectrometry (MIKES)-MS/MS was found to be much less selective than the TSQ-MS/MS for the analysis of nitro-PAH in unfractionated diesel extracts. HPLC prefractionation was required to remove interferences in the MIKES analysis. Fused silica capillary GC/MS using on-column injection was found to be necessary for identifying specific nitro-PAH isomers and minimizing decomposition. The highly mutagenic 1-nitropyrene (1-NP) was the only compound found in the nitro(pyrenes and fluoranthenes) isomer group. The MIKES and TSQ techniques gave comparable results for the quantitation of 1-NP.