Journal
ANALYTICAL CHEMISTRY
Volume 83, Issue 24, Pages 9531-9539Publisher
AMER CHEMICAL SOC
DOI: 10.1021/ac202317m
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Funding
- National Institutes of Health (NIH) [GM054585-15]
- National Science Foundation (NSF) [CHE-0911330]
- Agilent Foundation
- ANPCyT-UNLP (Argentina)
- Division Of Chemistry
- Direct For Mathematical & Physical Scien [0911516] Funding Source: National Science Foundation
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The use of flow splitters between the two dimensions in online comprehensive two-dimensional (2D) liquid chromatography (LC x LC) has not received very much attention, in comparison with their use in 2D gas chromatography (GC x GC), where they are quite common. In principle, splitting the flow after the first dimension column and performing online LC x 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 perform 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 through the 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, 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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