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Highly Sensitive Determination of 246-Trinitrotoluene and Related Byproducts Using a Diol Functionalized Column for High Performance Liquid Chromatography

机译:使用Diol官能化色谱柱高效灵敏地测定246-三硝基甲苯及相关副产物

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摘要

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.
机译:在这项工作中,一种用于完全分离2,4,6-三硝基甲苯(TNT)的新检测方法。 2,4-二硝基甲苯(2,4-DNT); 2,6-二硝基甲苯(2,6-DNT);使用二醇色谱柱开发了具有紫外传感器的高效液相色谱(HPLC)中的2-氨基二硝基甲苯(2-ADNT)和4-氨基二硝基甲苯(4-ADNT)分子。与现有方法相比,此方法可提高成本,时间和灵敏度,从而提供一种简单有效的替代方法。包括运行之间的色谱柱重新平衡在内的总分析时间少于13分钟,其中使用水和乙腈作为梯度洗脱溶剂。在优化的条件下,2,4-DNT和2,6-DNT峰之间的最小分辨率为2.06。加标环境样品的回收率在95–98%之间。 TNT及其副产物的二醇柱检出限为0.78至1.17 µg / L。虽然两相EPA的溶剂消耗量为26.4 mL / min,而EPA 8330方法的溶剂消耗量为30 mL / min,但二醇柱的消耗量仅为8.8 mL / min。相对于两相EPA和EPA 8330方法,分辨率提高了49%。与C-18和苯基-3色谱柱相比,使用二醇色谱柱可将溶剂用量降低多达64%,并且分离度提高了约两倍。二醇柱的灵敏度是由多元醇层上的羟基提供的,根据受体-供体之间的相互作用,电荷转移配合物与硝基芳族化合物形成了结合。符合当前要求,所提出的方法证明了灵敏且牢固的分离。

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