Effect of sampling rate on resolution in comprehensive two-dimensional liquid chromatography
Effect of sampling rate on resolution in comprehensive two-dimensional liquid chromatography
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DOI：
10.1021/ac971184b
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发表时间：
1998-04-15
影响因子：
7.4
通讯作者：
Foley, JP
中科院分区：
文献类型：
--
作者：
Murphy, RE;Schure, MR;Foley, JP
在“综合”二维液相色谱中，来自第一分离系统（第一维）的柱流出物通过第二维分离系统顺序取样。总分析时间主要由第二维分离系统的速度决定;保留最多的组分必须在下一个第二维分离的保留最少的组分之前分离。多维分离系统的优化要求人们理解系统分辨率与第一维峰上的第二维样品数量之间的关系。在本文中，我们研究了这种采样过程的理论和实验方面。为了获得高的二维分辨率，当采样是同相的时，第一维中的每个峰应当被采样到第二维中至少三次。如果采样是最大异相的，则每个峰至少应有四个样本以进行高保真分离。详细讨论了相对于采样相位的分辨率的灵敏度，并且当在第一维度峰宽上取四个或更多个样本时，所述灵敏度被示出为无关紧要。这些结果为多维色谱法的方法开发提供了最佳标准。
In "comprehensive" two-dimensional liquid chromatography, the column effluent from the first separation system (the first dimension) is sequentially sampled by the second dimension separation system. The total analysis time is largely determined by the speed of the second dimension separation system; the most retained component must elute before the least retained component of the next second dimension separation. Optimization of multidimensional separation systems requires that one understand the relationship between system resolution and the number of second dimension samples across a first dimension peak. In this paper, we study the theoretical and experimental aspects of this sampling process. To obtain high two-dimensional resolution, each peak in the first dimension should be sampled at least three times into the second dimension when the sampling is in-phase. If the sampling is maximally out of phase, there should be at least four samples per peak for high-fidelity separation. The sensitivity of the resolution with respect to the sampling phase is discussed in detail and shown to be insignificant when four or greater samples are taken across the first dimension peak width. These results suggest optimal criteria for method development with multidimensional chromatography.