Determination of N-nitroso derivatives of hexahydro-1,3,5-trinitro-1,3,5- triazine (RDX) in soils by pressurized liquid extraction and liquid chromatography-electrospray ionization mass spectrometry

Xiaoping Pan, Baohong Zhang, Stephen B. Cox, Todd A. Anderson, George P. Cobb

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46 Scopus citations

Abstract

To aid in the evaluation of the potential toxicity of N-nitroso derivatives of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX), we describe a pressurized liquid extraction (PLE) followed by liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) method for determination of RDX and its N-nitroso derivatives: hexahydro-1-nitroso-3,5-dinitro-1,3,5-triazine (MNX), hexahydro-1,3-dinitroso-5-nitro-1,3,5-triazine (DNX), and hexahydro-1,3,5- trinitroso-1,3,5-triazine (TNX) in soils. Sandy loam soil was spiked with RDX and its N-nitroso derivatives (MNX, DNX, and TNX). Acetonitrile was used as the PLE extraction solvent at 100°C and 1500 psi for 15 min. Florisil was used to cleanup extracts following PLE. Instrumental analysis employed LC-ESI-MS, in which 1 mM acetic acid was added to the mobile phase to facilitate formation of acetate adduct ions [M + CH3COO]-. The method detection limits (MDLs) for RDX, MNX, DNX, and TNX were 1.46, 1.46, 1.69, and 1.93 ng/g, respectively. High recovery (91.1-108.3%), good precision (RSD: 3.2-12.4%), and reproducibility were achieved. This method proved effective and was applied to monitor the reductive biotransformation of MNX in soils with the presence of earthworms (Eisenia fetida).

Original languageEnglish
Pages (from-to)2-8
Number of pages7
JournalJournal of Chromatography A
Volume1107
Issue number1-2
DOIs
StatePublished - Feb 24 2006

Keywords

  • DNX
  • ElectroSpray ionization (ESI)
  • Explosives
  • Liquid chromatography (LC)
  • MNX
  • Mass spectrometry (MS)
  • N-Nitroso compounds (NOCs)
  • Pressurized liquid extraction (PLE)
  • RDX
  • Soil
  • TNX

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