title: Highly sensitive determination of 2,4,6-trinitrotoluene and related byproducts using a diol functionalized column for high performance liquid chromatography.
abstract: In this work, a new detection method for complete separation of 2,4,6-trinitrotoluene (TNT); 2,4-dinitrotoluene (2,4-DNT); 2,6-dinitrotoluene (2,6-DNT); 2-aminodinitrotoluene (2-ADNT) and 4-aminodinitrotoluene (4-ADNT) molecules in high-performance liquid-chromatography (HPLC) with UV sensor has been developed using diol column. This approach improves on cost, time, and sensitivity over the existing methods, providing a simple and effective alternative. Total analysis time was less than 13 minutes including column re-equilibration between runs, in which water and acetonitrile were used as gradient elution solvents. Under optimized conditions, the minimum resolution between 2,4-DNT and 2,6-DNT peaks was 2.06. The recovery rates for spiked environmental samples were between 95-98%. The detection limits for diol column ranged from 0.78 to 1.17 µg/L for TNT and its byproducts. While the solvent consumption was 26.4 mL/min for two-phase EPA and 30 mL/min for EPA 8330 methods, it was only 8.8 mL/min for diol column. The resolution was improved up to 49% respect to two-phase EPA and EPA 8330 methods. When compared to C-18 and phenyl-3 columns, solvent usage was reduced up to 64% using diol column and resolution was enhanced approximately two-fold. The sensitivity of diol column was afforded by the hydroxyl groups on polyol layer, joining the formation of charge-transfer complexes with nitroaromatic compounds according to acceptor-donor interactions. Having compliance with current requirements, the proposed method demonstrates sensitive and robust separation.
authors.affiliation: UNAM, Institute of Materials Science and Nanotechnology, Bilkent University, Ankara, Turkey; MESA+ Institute for Nanotechnology, University of Twente, Enschede, the Netherlands.
authors.forename: Burcu
authors.initials: B
authors.lastname: Gumuscu
authors.affiliation: UNAM, Institute of Materials Science and Nanotechnology, Bilkent University, Ankara, Turkey.
authors.forename: Zeynep
authors.initials: Z
authors.lastname: Erdogan
authors.affiliation: UNAM, Institute of Materials Science and Nanotechnology, Bilkent University, Ankara, Turkey.
authors.forename: Mustafa O
authors.initials: MO
authors.lastname: Guler
authors.affiliation: UNAM, Institute of Materials Science and Nanotechnology, Bilkent University, Ankara, Turkey; Life Sciences Application and Research Center, Gazi University, Ankara, Turkey; Department of Medical Biology and Genetics, Faculty of Medicine, Gazi University, Ankara, Turkey.
authors.forename: Turgay
authors.initials: T
authors.lastname: Tekinay
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods; D012680:Sensitivity and Specificity; D014303:Trinitrotoluene / Q000032:analysis* / Q000737:chemistry*
chemical_list: D014303:Trinitrotoluene