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PH05 Fate and Effects of Energetic Compounds
(PH033) SPE Method Development and HPLC Determination of Explosives in Environmental Media.
Pan, X1, Smith, J1, Cobb, G1, 1 Texas Tech University, Lubbock, TX, USA
ABSTRACT- This study aims to develop a reproducible and sensitive method to measure trace explosive compounds and their transformation products. First, an HPLC method for the baseline separation of the 8 explosive compounds in a matrix-free sample is developed. Then, an optimal SPE method for analyte isolation from samples is established. This method requires: 1) adding salt to increase the ionic strength of the samples; 2) extra dying time to facilitate analyte recovery by acetonitrile. Recoveries of TNX using C18 were 68.5±8.4%, 83.2±5.2% and 90.5±6.4% at concentrations of 1ng/ml, 5ng/ml and 10ng/ml, respectively. Recoveries of RDX using C18 were 82.5±5.2% and 90.7±8.1% at concentrations of 1ng/ml and 20ng/ml, respectively. Recoveries of TNX using styrene-divinybenzene cartridge (SDB) were 91.2±14.4%, 96.5±13.1% and 99.0±6.3% at concentrations of 1ng/ml, 5ng/ml and 10ng/ml, respectively. Recoveries of RDX using SDB were 93.0±4.0% and 96.5±6.2% at concentrations of 1ng/ml and 20ng/ml, respectively. Additionally, good peak shape was achieved by diluting the acetonitrile extract with water. This method is currently applied for dose verification of an animal exposure study. The nominal TNX concentrations in water were 1, 10 and 100 ng/ml. In 17 replicates for each dose, our method produced the mean concentration of 0.91±0.15ng/ml, 10.0±1.0ng/ml and 100.3±8.4ng/ml, respectively. Future application will include tissue samples.
Key words: Explosive, TNX, SPE, HPLC
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