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Ionic Liquid Stationary Phase for Improving Comprehensive Two-dimensional Gas Chromatographic Separation of Polychlorinated Naphthalenes
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2020-11-26 , DOI: 10.1016/j.chroma.2020.461732
J.F. Ayala-Cabrera , C. Lipok , J. Li , E. Moyano , O.J. Schmitz , F.J. Santos

The performance of comprehensive two-dimensional gas chromatography coupled to mass spectrometry (GC×GC-MS) using a column combination of a non-polar stationary phase (DB-5MS) and an ionic liquid stationary phase (SLB-IL60) in the first- and the second dimension has been evaluated for the suitable separation of polychlorinated naphthalenes (PCNs). The optimization of the GC×GC-MS method was carried out using different oven temperature programs and modulation conditions, achieving the best results using a ramp temperature rate of 0.75 °C min−1 and a modulation time of 12 s. Under these conditions, efficient separation of all PCN congeners present in Halowax formulations was achieved in 140 min, resolving some critical closed eluting isomers, such as CN-33/34/37, highly toxic CN-66/67 or CN-71/72 pairs, among others. These findings represent a significant improvement in the congener-specific separation of PCNs over the 1D-GC and GC×GC methodologies already published and the DB-5MS × SLB-IL60 column combination offered the orthogonality required for the congener-specific determination with a high peak capacity. The GC×GC-MS method was applied to the characterisation of Halowax formulations, obtaining similar compositional profiles than those previously reported.



中文翻译:

离子液体固定相可改善多氯萘的二维气相色谱综合分离

首次使用非极性固定相(DB-5MS)和离子液体固定相(SLB-IL60)的色谱柱组合进行全面二维气相色谱-质谱联用(GC×GC-MS)的性能-已经对第二维进行了多氯代萘(PCN)的合适分离的评估。使用不同的柱箱温度程序和调制条件对GC×GC-MS方法进行了优化,使用0.75°C min -1的升温速率可获得最佳结果调制时间为12 s。在这些条件下,可在140分钟内有效分离Halowax制剂中存在的所有PCN同系物,从而解决了一些关键的封闭洗脱异构体,例如CN-33 / 34/37,高毒性CN-66 / 67或CN-71 / 72对,等等。这些发现表明,与已经发表的一维气相色谱和气相色谱×GC方法相比,PCN的同族特异性分离有了显着改善,并且DB-5MS×SLB-IL60色谱柱组合提供了高同族特异性测定所需的正交性。峰值容量。将GC×GC-MS方法应用于Halowax制剂的表征,获得了与先前报道的相似的组成曲线。

更新日期:2020-12-04
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