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
1. [1]
  [1] Yu S L. Methods and Applications of High Performance Liquid Chromatography. Beijing: Chemical Industry Press (于世林. 高效液相色谱方法及应用. 北京: 化学工业出版社), 2000: 4, 8
2. [2]
  [2] Jiang S X, Liu X. Science in China (Series B): Chemistry (蒋生祥, 刘霞. 中国科学(B辑): 化学), 2009, 39(8): 687
3. [3]
  [3] Mullangi R, Sharma K, Srinivas N R. Biomed Chromatogr, 2012, 26(8): 906
4. [4]
  [4] Shen A J, Guo Z M, Liang X M. Progress in Chemistry (沈爱金, 郭志谋, 梁鑫淼. 化学进展), 2014, 26(1): 10
5. [5]
  [5] Jardim I C S F, Maldaner L, Lourenco J, et al. J Sep Sci, 2010, 33(19): 2917
6. [6]
  [6] Tan Y, Fan J, Lin C, et al. J Sep Sci, 2014, 37(5): 488
7. [7]
  [7] McCalley D V. J Chromatogr A, 2010, 1217(6): 858
8. [8]
  [8] da Silva C G A, Collins C H. J Chromatogr A, 2012, 1260: 81
9. [9]
  [9] Huang X J, Yang X L, Liu X L, et al. Chemical Reagents (黄晓佳, 杨新立, 刘学良, 等. 化学试剂), 2001, 23(2): 77
10. [10]
  [10] Chen H M, Li L S, Ma H P, et al. Chinese Journal of Analysis Laboratory (陈会明, 李来生, 马海萍, 等. 分析试验室), 2010, 29(3): 14
11. [11]
  [11] Chen H, Li L S, Zhang Y, et al. Chinese Journal of Chromatography (陈红, 李来生, 张杨, 等. 色谱), 2012, 30(10): 1062
12. [12]
  [12] Zhang Y, Liu M F, Fang Y S, et al. Journal of Nanchang University: Natural Science (张杨, 刘妙芬, 方奕姗, 等. 南昌大学学报: 理科版), 2012, 36(3): 228
13. [13]
  [13] Fang Y S, Li L S, Chen H, et al. Chinese Journal of Applied Chemistry (方奕珊, 李来生, 陈红, 等. 应用化学), 2013, 30(1): 79
14. [14]
  [14] Pharmacopoeia Committee of the Ministry of Public Health of the People's Republic of China (PRC). National Pharmaceutical Standard of Ministry of Public Health of PRC: Preparation of Chinese Medicine, Part 9. Beijing: Chemical Industry Press (中华人民共和国卫生部药典委员会. 中华人民共和国卫生部药品标准: 中药成方制剂, 第9册. 北京: 化学工业出版社), 1994: 42
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沈阳化工大学材料科学与工程学院沈阳 110142