Use of solid-phase microextraction/gas chromatography-election capture detection for the determination of energetic chemicals in marine samples

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DOIResolve DOI: http://doi.org/10.1016/j.chroma.2005.01.049
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TypeArticle
Journal titleJournal of Chromatography A
Volume1066
Issue1-2
Pages177187; # of pages: 11
Subjectenv
AbstractGas chromatography with electron capture detection (GC-ECD) is a highly explosive-sensitive analytical technique. However, its application to the analysis of sediment extracts is hampered by the presence of numerous endogenous interferences. In the present study, solid-phase microextraction (SPME) was used both as a purification technique for sediment extracts and as an extraction technique for water samples prior to analysis by GC-ECD. SPME/GC-ECD coupling was optimized and applied to the trace analysis of nine explosives including nitroaromatics and RDX in real seawater and marine sediment samples. Addition of a high concentration of salt (30%, w/v) in the aqueous medium and use of a carbowax/divinylbenzene (CW/DVB) coating led to optimal extraction efficiencies. Method detection limits (MDLs) ranged from 0.05 to 0.81 ?g/L in water and from 1 to 9 ?g/kg in dry sediment. Except for RDX, spike recoveries in seawater were satisfactory (89-147%) when samples were fortified at 2 ?g/L of each analyte. Spike recoveries from dry sediment fortified at 10 ?g/kg of each analyte gave lower recoveries but these could also be due to degradation in the matrix. With a smaller volume of aqueous sample required compared to solid-phase extraction (SPE), SPME is an attractive method for the analysis of limited volumes of sediment pore-water. Moreover, the use of SPME eliminated interferences present in sediment extracts thus allowing the detection of the target analytes that were otherwise difficult to detect by direct injection.
Publication date
LanguageEnglish
AffiliationNRC Biotechnology Research Institute; National Research Council Canada
Peer reviewedNo
NRC number47224
NPARC number3539775
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Record identifier9f9df265-6f32-4581-b832-a72262c97252
Record created2009-03-01
Record modified2016-05-09
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