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A pH-stable, crosslinked stationary phase based on the thiol-yne reaction.

Journal of chromatography. A (2019-04-15)
Erin P Shields, Stephen G Weber
ABSTRACT

Stationary phases that can withstand extremes of pH and temperature are needed to allow a single column to accommodate a wider set of solutes and separation criteria. We used a simple multi-step process using the thiol-yne reaction following the modification of the silica surface with a thiol-containing silane. The monomers 1,4-diethynylbenzene (DEB) and 1,6-hexanedithiol were used to create a crosslinked thiol-yne (CTY) stationary phase along the surface of the thiol functionalized silica. In the Tanaka test characterization, the CTY phase showed a low phase ratio, methylene selectivity typical of a reversed phase, and extremely high shape selectivity compared to commercial reversed phases. The hydrophobic subtraction model characterization showed a high positive steric resistance, a low hydrogen bond acidity, and a high cation-exchange capacity compared to most reversed phases. At pH 0.5 with an 85% aqueous mobile phase the phase showed no significant change over 114 h. With a 50% aqueous mobile phase the phase took four more days than a sterically protected C18 phase for the k' to decline 25%. At pH 12.6, 50% aqueous mobile phase, a sterically protected C18 phase showed a 20% decrease in k' and more than a 60% decrease in theoretical plates per meter in three hours. The CTY phase actually showed modest increases in k' and theoretical plates per meter after three hours.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
(3-Mercaptopropyl)trimethoxysilane, 95%
Sigma-Aldrich
Octanophenone, ≥99%
Sigma-Aldrich
Heptanophenone, 98%

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