Liquid chromatography (LC) is a robust and universal analytical method for the separation of compounds, making it a widely-used technique in fields from pharmaceuticals to environmental science. With the growing complexity of samples, improved resolution is needed for better quantitation. For the past couple of decades, chromatographers have focused on refining the efficiency of the stationary phase. Optimization of the selectivity of the stationary phase is an underutilized approach towards improving resolution. Previous work has shown that this can be done with the creation of a continuous gradient along the length of the column. This work focuses on the development of a destructive gradient stationary phase, where the functional groups on a commercially packed column are cleaved using controlled rate infusion to form a gradient along the length of the column. Preliminary experiments demonstrate a change in the retention factors for the probe analytes being studied along with a change in elution order indicating a possible change in retention mechanism for the compounds. These results show that C<sub>4</sub> functional groups can be cleaved with the use of sulfuric acid, thus changing the selectivity of the stationary phase. Ongoing work is focused on characterizing the destructive gradient though Raman spectroscopy, and studying the reproducibility of this technique. We believe that this strategy has promise as being a controllable and precise way of creating a gradient on a commercially available column.

Destructive stationary phase gradients for liquid chromatography

254th National Meeting (2017)

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