Improving peak capacity in fast online comprehensive two-dimensional liquid chromatography with post-first-dimension flow splitting.

Improving peak capacity in fast online comprehensive two-dimensional liquid chromatography with post-first-dimension flow splitting.
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DOI:
10.1021/ac202317m
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发表时间:
2011-12-15
影响因子:
7.4
通讯作者:
Carr, Peter W.
Carr, Peter W.
中科院分区:
化学1区
文献类型:
--
作者:
Filgueira, Marcelo R.;Huang, Yuan;Witt, Klaus;Castells, Cecilia;Carr, Peter W.

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在线综合二维液相色谱(LC×LC)中二维分流器的使用,与GC×GC中常见的二维分流器相比,还没有引起足够的重视。原则上,在第一维度柱之后分流并对第一维度流出物的该恒定分数进行在线LC×LC应允许几乎独立地优化两个维度。当没有分流时,第一维度流速的任何变化对第二维度具有直接影响。利用分流器,可以例如使进入第一维柱的流速加倍,并且进行1:1分流,而不改变样品环尺寸或采样器的收集时间。当然,灵敏度会降低,但这可以通过使用更大的注入来部分补偿;这可能仅相当于为这种增加的分辨率和系统灵活性付出的很小代价。在其他益处中,我们发现通过使用后第一维分流器,校正的2D峰容量和观察到的峰的数量在15分钟的分析时间内增加了2倍。在固定的分析时间,这种改善主要是由于减少系统再平衡时间导致的梯度时间增加,并且在较小程度上是由于通过第一维的完全优化实现的峰容量增加。
The use of flow splitters between the two dimensions in on-line comprehensive two dimensional liquid chromatography (LC×LC) has not received very much attention in comparison to their use in GC×GC where they are quite common. In principle, splitting the flow after the first dimension column and performing on-line LC×LC on this constant fraction of the first dimension effluent should allow the two dimensions to be optimized almost independently. When there is no flow splitting any change in the first dimension flow rate has an immediate impact on the second dimension. With a flow splitter one could for example double the flow rate into the first dimension column and do a 1:1 flow split without changing the sample loop size or the sampler’s collection time. Of course, the sensitivity would be diminished but this can be partially compensated by use of a larger injection; this will likely only amount to a small price to pay for this increased resolving power and system flexibility. Among other benefits, we found a 2-fold increase in the corrected 2D peak capacity and the number of observed peaks for a 15 min analysis time by using a post first dimension flow splitter. At a fixed analysis time this improvement results primarily from an increase in the gradient time resulting from the reduced system re-equilibration time and to a smaller extent it is due to the increased peak capacity achieved by full optimization of the first dimension.
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