Synthesis and Characterization of Amino‐Based Columns for HPLC Made by Silanization/Hydrosilation

Abstract

Synthesis and characterization of amino‐based stationary phases for high performance liquid chromatography is described. The amino‐based stationary phases for HPLC have been synthesized following a silanization/hydrosilation method. Three organic compounds, N‐(3‐butynyl) phthalimide, 4‐diethylamino‐2‐butyn‐1‐ol, and 3‐amino‐3‐methyl‐1‐butyne were chosen as bonding moieties for the hydrosilation reaction. The synthesized bonded phases were characterized by cross polarization magic angle spinning nuclear magnetic resonance (CP MAS‐NMR), diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy, and elemental analysis. Chromatographic evaluation of the bare silica, silica hydride, endcapped silica hydride, N‐(3‐butynyl) phthalimide phase, amino phase via cleavage of N‐(3‐butynyl) phthalimide phase (4‐amino‐1‐butyne phase), and 3‐amino‐3‐methyl‐1‐butyne bonded phases was done by sugar analysis.

Keywords:

• Amino‐based columns
• HPLC
• Silanization/hydrosilation
• Synthesis
• Characterization

Acknowledgments

The authors wish to thank the National Science Foundation (Grant CHE 0094983) and the National Institutes of Health (Grant R15 GM 63519‐01) for support of the research reported here. Special thanks to Eka Nobel AB (Sweden) for donation of Kromasil silica.