TY - JOUR
T1 - 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
AU - Pan, Xiaoping
AU - Zhang, Baohong
AU - Cox, Stephen B.
AU - Anderson, Todd A.
AU - Cobb, George P.
N1 - Funding Information:
This work was funded by the Strategic Environmental Research & Development Program (SERDP), project no. CU1235. Lab assistance provided by Haitao Luo, Qingsong Cai, and Jun Liu is highly appreciated.
PY - 2006/2/24
Y1 - 2006/2/24
N2 - 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).
AB - 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).
KW - DNX
KW - ElectroSpray ionization (ESI)
KW - Explosives
KW - Liquid chromatography (LC)
KW - MNX
KW - Mass spectrometry (MS)
KW - N-Nitroso compounds (NOCs)
KW - Pressurized liquid extraction (PLE)
KW - RDX
KW - Soil
KW - TNX
UR - http://www.scopus.com/inward/record.url?scp=31844432366&partnerID=8YFLogxK
U2 - 10.1016/j.chroma.2005.12.025
DO - 10.1016/j.chroma.2005.12.025
M3 - Article
C2 - 16387311
AN - SCOPUS:31844432366
SN - 0021-9673
VL - 1107
SP - 2
EP - 8
JO - Journal of Chromatography A
JF - Journal of Chromatography A
IS - 1-2
ER -