Citation: XU Lili, REN Nailin, LIN Zeling. Preparation and application of an emodin-bonded silica gel chromatographic column for high performance liquid chromatography[J]. Chinese Journal of Chromatography, ;2014, 32(8): 798-803. doi: 10.3724/SP.J.1123.2014.04038 shu

Preparation and application of an emodin-bonded silica gel chromatographic column for high performance liquid chromatography

1.
Department of Chemistry, Hanshan Normal University, Chaozhou 521041, China

Corresponding author: XU Lili,
Received Date: 23 April 2014
Available Online: 23 June 2014
Fund Project: 韩山师范学院青年项目(LQ200906) (LQ200906)潮州市科技引导计划项目(2013H04). (2013H04)

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.
- high performance liquid chromatography (HPLC),
- bonded silica gel stationary phase,
- emodin ligand,
- chromatographic column,
- preparation,
- application
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沈阳化工大学材料科学与工程学院沈阳 110142