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Separation performance of dithienyl benzothiadiazole-based stationary phases for capillary gas chromatography

机译:二噻吩基苯并噻二唑基固定相的毛细管气相色谱分离性能

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This work explored the separation performance of two new dithienyl benzothiadiazole (TBT)-based materials, namely 4,7-di(5-allyl-2-thienyl)benzothiadiazole (TBT-AA) and 4-(5-allyl-2-thienyl)-7-(5-dodecyl-2-thienyl)benzothiadiazole (TBT-AC12), as the stationary phases for capillary gas chromatography (GC). The TBT-AA and TBT-AC12 columns exhibited medium polarity and achieved a column efficiency of 3700 plates?per m and 3800 plates per m, respectively, by n-dodecane under 100 °C. They showed high-resolution performance for analytes of different varieties and advantageous resolving capability for positional and structural isomers, such as chloronitrobenzenes, dibromobenzenes, cymenes and hexanes, over the polysiloxane stationary phase with similar polarity. Moreover, the TBT-based stationary phases display different retention behaviours from the conventional phase via diversified molecular interactions covering π–π and π–π EDA, halogen-bonding, H-bonding interactions and van der Waals forces. Also, they exhibited good column repeatability with the relative standard deviation (RSD) values of less than 0.12% for run-to-run, 1.8% for day-to-day and 5.0% for column-to-column, respectively. This work demonstrates the good potential of the TBT-based stationary phases for GC separations.
机译:这项工作探索了两种新的基于二噻吩基苯并噻二唑(TBT)的材料的分离性能,即4,7-二(5-烯丙基-2-噻吩基)苯并噻二唑(TBT-AA)和4-(5-烯丙基-2-噻吩基) )-7-(5-十二烷基-2-噻吩基)苯并噻二唑(TBT-AC12),作为毛细管气相色谱(GC)的固定相。 TBT-AA和TBT-AC12色谱柱表现出中等极性,在100°C下通过 n -十二烷分别获得3700板/ m和3800板/ m的柱效率。他们显示了具有不同极性的分析物的高分辨率性能,以及在极性相似的聚硅氧烷固定相上对位置和结构异构体(如氯硝基苯,二溴苯,苏木精和己烷)具有出色的分辨能力。此外,基于TBT的固定相通过覆盖π–π和π–π EDA的多种分子相互作用,卤素键,H键相互作用和范德华力,表现出与常规相不同的保留行为。 。而且,它们表现出良好的色谱柱重复性,相对于运行的相对标准偏差(RSD)值分别小于0.12%,日常的1.8%和小于柱间的5.0%。这项工作证明了基于TBT的固定相在气相色谱分离中的巨大潜力。

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