Analytical method for determination of dinitropyrenes using gas chromatography-high-resolution mass spectrometry

A gas chromatography-high-resolution mass spectrometry method has been developed for the determination of dinitropyrenes (DNPs). DNPs were reduced to the corresponding diaminopyrenes with sodium hydrosulfide, and the reduced DNPs were derivatized with N-metbylbis(trifluoroacetamide). The sensitivity of this method was up to 10 times that of high-performance liquid chromatography with fluorescence detection. The detection limits for 1,3-, 1,6-, and 1,8-DNPs were in the 0.90-1.1 pg range. The concentrations were corrected with a correction factor determined from the recovery of an internal standard. The recovery of deuterium-labeled 6-nitrochrysene was at least 87%. This new method was utilized for quantitative determination of DNPs in Standard Reference Material (SRM) 1975 available from the US National Institute of Standards and Technology. Three DNP isomers were measured in SRM 1975 at 0.571-1.59 mu g/g. (c) 2007 Elsevier B.V. All rights reserved.