Abstract
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.
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