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Observation and explanation of two-dimensional interconversion of oximes with multiple heart-cutting using comprehensive multidimensional gas chromatography
Journal of Chromatography A ( IF 3.8 ) Pub Date : 2018-02-21 , DOI: 10.1016/j.chroma.2018.02.035
Chadin Kulsing , Yada Nolvachai , Yong Foo Wong , Melissa I. Glouzman , Philip J. Marriott

Real-time interconversion processes produce unconventional peak broadening in gas chromatography (GC), and can be used to generate kinetic and thermodynamic data. In this study, an unusual separation situation in comprehensive two dimensional GC where two dimensional interconversion (i.e. a raised plateau in both first and second dimension, 1D and 2D) was observed in analysis of oxime isomers. This resulted in a characteristic and unusual rectangular peak shape in the two dimensional result. A related theoretical approach was introduced to explain the peak shape supported by simulation results which can be varied depending on concentration profiles and kinetics of the process. The simulated results were supported by experimental results obtained by a comprehensive heart-cut multidimensional GC (H/C MDGC) approach which was developed to clearly investigate isomerisation of E/Z oxime molecules in both 1D and 2D separations under different isothermal conditions. The carrier gas flow and oven temperature were selected according to initial results for 1D interconversion on a poly(ethyleneglycol) stationary phase, which was further used in both 1D and 2D separations to result in broad zones of oxime interconversion in both dimensions. The method involved repetitive injections of oxime sample, then sampling contiguous fractions of sample into a long 2D column which is intended to promote considerable interconversion. Comprehensiveness arises from the fact that the whole sample is sampled from the 1D to the 2D column, with the long 2D column replacing the short 2D column used in classical comprehensive two-dimensional gas chromatography, where the latter will not promote sufficient interconversion. Data processing and presentation permits a ‘rectangular’ distribution corresponding to the separated compounds, characteristic of this experiment.



中文翻译:

综合多维气相色谱法对肟进行多中心切割二维相互转化的观察和解释

实时互转换过程在气相色谱(GC)中产生非常规的峰展宽,可用于生成动力学和热力学数据。在这项研究中,在综合二维GC一个不寻常的分离情况,其中二维互变(一个在第一和第二维凸起的平台,1 d和2D)在肟异构体的分析中观察到。这在二维结果中产生了特征性且不寻常的矩形峰形。引入了一种相关的理论方法来解释模拟结果所支持的峰形,该峰形可以根据浓度曲线和过程动力学而变化。模拟的结果通过由被开发来调查清楚的异构化的综合性心脏切多维GC(H / C MDGC)的方法得到的实验结果的支持E / Z肟分子中既1 d和2不同等温条件下的D分离。载气流和烘箱温度是根据用于在聚(乙二醇)固定相1D的相互转换,其在两个进一步使用初始结果中选择1 d和2层d的分离导致在两个维度肟互变的广阔区域。该方法包括重复注入肟样品,然后将样品的连续馏分采样到一个长的2 D色谱柱中,以促进可观的相互转化。全面性源于以下事实:整个样品都从1 D到2 D色谱柱采样,而长2 D色谱柱代替了短2色谱柱D柱用于经典的全面二维气相色谱法中,后者不会促进足够的相互转化。数据处理和表示允许“矩形”分布与分离的化合物相对应,这是该实验的特征。

更新日期:2018-02-21
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