关键词: 大黄素配体, 高效液相色谱, 键合硅胶固定相, 色谱柱, 应用, 制备

Abstract:

An emodin-bonded silica gel stationary phase (ESP) for high performance liquid chromatography has been synthesized by the intermediate method. The preparation process was as follows:γ-glycidoxypropyltrimethoxy silane (KH-560) firstly reacted with emodin ligand; then the intermediate was chemically immobilized to the surface of silica gel. Characterization of ESP was carried out with Fourier transform infrared spectroscopy (FTIR), elemental analysis and thermogravimetric analysis. Naphthalene was used as a probe to determine the column efficiency with methanol-water (60:40, v/v) as binary mobile phase at a flow rate of 0.8 mL/min. In order to elucidate the related separation mechanism, ESP was used to separate a series of neutral, basic and acidic aromatic compounds, as well as a sample of wind medicated oil. The conventional C₁₈ column and phenyl column were also tested under the same chromatographic conditions for comparison. The results showed that the emodin ligand was successfully bonded to the surface of spherical silica gel with a 0.23 mmol/g of bonded amount, and the theoretical plate number of ESP column was about 19874 N/m. The coupling reagent chains and anthraquinone rings in ESP offered a structural basis for hydrophobic interaction. Meanwhile, the emodin ligands provided π-π or p-π, charge transfer, hydrogen bonding, dipole-dipole action sites for different analytes. The synergistic reaction of various action sites endowed ESP column special and excellent chromatographic separation selectivity. And a baseline separation of polar compounds such as amines and phenols on ESP was easily achieved by using common and cheap methanol-water mobile phases without buffer salts. The experimental conditions were simple and convenient.

Key words: application, bonded silica gel stationary phase, chromatographic column, emodin ligand, high performance liquid chromatography (HPLC), preparation