Department of Chemistry, University of Washington, Box 351700, Seattle, WA 98195, USA.
Department of Chemistry, University of Washington, Box 351700, Seattle, WA 98195, USA; Department of Chemistry and Life Science, United State Military Academy, West Point, NY 10996.
Talanta. 2019 Apr 1;195:822-829. doi: 10.1016/j.talanta.2018.12.007. Epub 2018 Dec 6.
The separation power of comprehensive three-dimensional gas chromatography (GC) is substantially enhanced through proper selection of the phase volume ratio, β, of each column relative to each other on successive dimensions. Consideration and application of the ratio of phase volume ratios, β, or β ratio, between successive dimensions has been a relatively un-studied approach to maximize separating power in comprehensive multidimensional GC instrument design. Herein, proper selection of β in multidimensional GC is shown to control the elution temperature, T, of analytes throughout a 40 min primary (D) column separation, and thus better control width-at-base, W, on all three dimensions. Specifically, between the D and secondary (D) columns, a β of 0.45 was applied, and between the D and tertiary (D) columns a β of 1.0 was applied. A total ideal peak capacity of 30,600, or a peak capacity production of 770 peaks/min, was accomplished with the GC instrument with the reconfigured parameters. Additionally, due to the complex nature of this three-dimensional data, a novel approach to "slicing" the chromatographic run into user-defined time intervals is shown. This novel way to view the data still elicits a traditional GC×GC chromatograms, but with the focus on D × D separations. Moreover, due to proper β selection, every 2 s window (i.e. every D modulation period) is shown to have a peak capacity of ~50-100 for each D × D separation. This high overall peak capacity (30,600) and peak capacity per D modulation (50-100), courtesy of proper column selection, is demonstrated to hold great promise to physically separate truly complex mixtures.
通过适当选择各柱之间的相体积比β,可以大大提高综合三维气相色谱(GC)的分离能力。考虑并应用各维度之间的相体积比β或β比,可以相对较少地研究最大限度地提高综合多维 GC 仪器设计中分离能力的方法。本文表明,在多维 GC 中适当选择β可以控制 40min 主(D)柱分离过程中分析物的洗脱温度 T,从而更好地控制所有三个维度上的峰底宽 W。具体来说,在 D 和次级(D)柱之间应用β=0.45,在 D 和三级(D)柱之间应用β=1.0。GC 仪器的参数重新配置后,实现了 30600 个理想的峰容量,或 770 个峰/分钟的峰容量产量。此外,由于这种三维数据的复杂性,本文还展示了一种将色谱运行“切片”为用户定义时间间隔的新方法。这种查看数据的新方法仍然会产生传统的 GC×GC 色谱图,但重点是 D×D 分离。此外,由于正确的β选择,每个 2s 窗口(即每个 D 调制周期)都显示出每个 D×D 分离的峰容量约为 50-100。这种高总体峰容量(30600)和每个 D 调制的峰容量(50-100),得益于正确的柱选择,有望在物理上分离真正复杂的混合物。