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Particles without a Box: Brush-first Synthesis of Photodegradable PEG Star Polymers under Ambient Conditions

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In-column bonded phase polymerization for improved packing uniformity.

Alexis G Huckabee¹, Charu Yerneni¹, Rachel E Jacobson¹

¹Department of Chemistry, Purdue University, West Lafayette, IN, USA.

Journal of Separation Science

|April 8, 2017

Summary

In situ polymer growth offers superior chromatographic performance and column stability compared to ex situ methods. This novel approach enhances resolution and reproducibility in chromatography by creating robust particle interactions.

Keywords:

glycoproteins hydrophilic interaction liquid chromatography packing polymer stationary phases

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Area of Science:

Chromatography
Polymer Chemistry
Materials Science

Background:

Packing chromatographic columns with polymeric-bonded phases is challenging due to polymer swelling in slurry solvents.
Conventional ex situ polymer growth methods can lead to suboptimal column performance and reproducibility.

Purpose of the Study:

To investigate and compare the performance of in situ versus ex situ polymer growth for chromatographic stationary phases.
To evaluate the impact of in situ polymer growth on chromatographic resolution, reproducibility, and column stability.

Main Methods:

Utilized activators generated by electron transfer and atom-transfer radical polymerization for ambient condition polymerization.
Employed nonporous silica particles with silane initiators for polyacrylamide film growth.
Assessed performance using hydrophilic interaction liquid chromatography (HILIC) with ribonuclease B and peak width analysis of acetonitrile.

Main Results:

Achieved comparable polyacrylamide film thickness and carbon coverage for both in situ and ex situ growth.
Demonstrated higher chromatographic resolution and column-to-column reproducibility with in situ growth.
Observed lower eddy diffusion and improved bed stability against collapse for in situ polymer growth.

Conclusions:

In situ polymer growth provides enhanced chromatographic resolution and stability compared to ex situ methods.
The improved performance is attributed to harder particle-particle contacts in columns packed with in situ grown polymers.
This method offers a more robust and reproducible approach for preparing chromatographic stationary phases.