Preparation of Poly(1-dodecene-co-trimethylol propane triacrylate-co-ethylene dimethacrylate) Monolithic Column for HPLC Separations of Small Molecules

Abstract

A new poly(1-dodecene-co-trimethylol propane triacrylate-co-ethylene dimethacrylate) [poly(C12-co-TMPTA-co-EDMA)] monolithic column was prepared via in situ free-radical polymerization reaction. Various parameters affecting the polymerization were investigated and optimized. The permeability of the monolithic column was calculated as 2.9098 × 10⁻¹⁴ m² with methanol as the mobile phase and the surface areas was 73.1 m²/g by the nitrogen adsorption–desorption experiment. The morphologies of the monolith were characterized by scanning electron microscopy (SEM) and the mechanical strength has been studied in detail as well. The prepared monolith was then used as the stationary phase of reversed phase high-performance liquid chromatography (RP-HPLC) to separate small molecule compounds. Column efficiency for chlorobenzene reached 14,340 theoretical plates per meter. The monolith also showed satisfactory reproducibility, based on the retention times of benzene, phenol, chlorobenzene, diphenylamine, and anthracene; the relative standard deviation (RSD) values for run-to-run, column-to-column and batch-to-batch were less than 0.62%, 3.2%, and 5.7%, respectively.

Keywords:

• good repeatability
• high-performance liquid chromatography
• monolithic column
• poly(C12-co-TMPTA-co-EDMA) monolith
• reversed-phase chromatography
• small molecules