Stationary phase based on cellulose dodecanoate physically immobilized on silica particles for high-performance liquid chromatography

Abstract

The chemical agent free preparation of a stationary phase using a natural macromolecule was the focus of this paper. Thermal immobilization of cellulose dodecanoate on silica particles was used for the preparation of a stationary phase without the use of chemical reagents. Cellulose modification was performed to produce a hydrophobic macromolecule with solubility in common organic solvents. The new stationary phase was characterized morphologically and physico-chemically, presenting as spherical particles immobilized with a thin cellulose dodecanoate layer. The degree of substitution of cellulose dodecanoate was 1.7, which resulted in a separation mechanism in reversed phase mode, but with lower hydrophobicity and higher steric selectivity, which are properties from cellulose. These characteristics resulted in a stationary phase with intrinsic selectivity that was able to separate mixtures of polar drugs, homologs of an anionic surfactant and omeprazole isomers, which are not well resolved in typical C18 phases. Considering that cellulose is a natural polymer and the preparation method of stationary phase involves only physical processes of silica modification, the final material presents as a stationary phase with specific retention properties coming from both dodecanoate and cellulose.