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基于两亲性三联苯的固定相用于高分辨气相色谱分离。

Amphiphilic triptycene-based stationary phase for high-resolution gas chromatographic separations.

机构信息

Key Laboratory of Cluster Science, Ministry of Education of China, School of Chemistry and Chemical Engineering, and Analysis & Testing Center, Beijing Institute of Technology, Beijing, 100081, China.

Key Laboratory of Cluster Science, Ministry of Education of China, School of Chemistry and Chemical Engineering, and Analysis & Testing Center, Beijing Institute of Technology, Beijing, 100081, China.

出版信息

J Chromatogr A. 2019 Aug 16;1599:239-246. doi: 10.1016/j.chroma.2019.04.033. Epub 2019 Apr 13.

Abstract

This work reports a new type of triptycene-based amphiphilic stationary phase (TP-2IL) for gas chromatography (GC). It is an integration of the 3D π-rich triptycene framework with ionic liquids. Its capillary column showed the efficiency of 3880 plates/m determined by n-dodecane at 120 °C (k = 2.79) and exhibited good performance for analytes from apolar to polar nature. Particularly, it has outstanding capability for resolving critical pairs of anilines and phenols with good peak shapes and shows distinct advantages over its composing counterparts (TP-2BO and O-IL) and widely-used commercial columns, namely 35% phenyl methyl polysiloxane (DB-35) and polyethylene glycol (INNOWAX). Moreover, the TP-2IL column exhibited good repeatability and reproducibility with the values of relative standard deviation in the range of 0.02%-0.07% for run-to-run, 0.10%-0.35% for day-to-day and 2.9%-5.1% for column-to-column, respectively, and good thermal stability up to 300 °C. Furthermore, its applications for determining isomer impurities in real samples demonstrate its feasibility for practical GC analysis. This work presents a facile strategy for constructing triptycene-based stationary phases with amphiphilic selectivity and provides alternatives of highly selective stationary phases for chromatographic analysis.

摘要

本工作报道了一种新型基于三并苯的两亲性固定相(TP-2IL)用于气相色谱(GC)。它是将三维富π的三并苯骨架与离子液体相结合。其毛细管柱在 120°C 下用正十二烷测定的效率为 3880 板/m(k=2.79),对从非极性到极性的分析物表现出良好的性能。特别是,它对苯胺和苯酚的关键对具有出色的分离能力,具有良好的峰形,与组成的对应物(TP-2BO 和 O-IL)和广泛使用的商业柱,即 35%苯基甲基聚硅氧烷(DB-35)和聚乙二醇(INNOWAX)相比具有明显的优势。此外,TP-2IL 柱具有良好的重复性和重现性,其运行间、日间和柱间的相对标准偏差分别在 0.02%-0.07%、0.10%-0.35%和 2.9%-5.1%范围内,热稳定性高达 300°C。此外,其在实际样品中测定异构体杂质的应用证明了其在实际 GC 分析中的可行性。本工作提出了一种构建具有两亲选择性的基于三并苯的固定相的简便策略,为色谱分析提供了高选择性固定相的替代品。

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