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Carbamic acid ester type liquid phase chromatogram stationary phase and preparation method thereof

A high-performance liquid chromatography and stationary phase technology, applied in the field of novel reversed-phase liquid chromatography stationary phase, can solve the problems of cumbersome preparation process of stationary phase, expensive reagents, etc., achieve good market application prospects, improve compatibility, and preparation process Simple and reliable effects

Active Publication Date: 2013-04-17
CHANGZHOU HIGH TECH RES INST OF NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the N-alkyl bonded chains prepared by this method are evenly distributed on the surface of silica gel and the batch preparation is reproducible, the preparation of the stationary phase is cumbersome and the reagents used are expensive.

Method used

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  • Carbamic acid ester type liquid phase chromatogram stationary phase and preparation method thereof
  • Carbamic acid ester type liquid phase chromatogram stationary phase and preparation method thereof
  • Carbamic acid ester type liquid phase chromatogram stationary phase and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 5 mL of propyltriethoxysilane isocyanate, 3 g of dodecanol and 40 mL of toluene into a 100 mL flask, heat to reflux for 3 hours, cool and dry for later use. Take another 2.5g of silica gel treated with hydrochloric acid in a 200mL flask, dry it in vacuum at 150°C for 5 hours, add the above reaction solution under vacuum drive, stir and reflux for 14 hours under the protection of nitrogen, filter, and wash with toluene and methanol successively. The obtained solid was dried in a vacuum oven at 80° C. for 12 hours to obtain a carbamate chromatographic stationary phase. Elemental analysis: C: 13.2%, N: 0.9%. Infrared spectrum: 2930 and 2858cm -1 Alkyl characteristic absorption peak, 1703cm -1 Carbonyl characteristic absorption peak, 1530cm -1 The characteristic absorption peak of the amide bond. The results of elemental analysis and infrared spectroscopy confirmed that the structure of the stationary phase is:

[0023]

Embodiment 2

[0025] Add 30mL of propyltriethoxysilane isocyanate, 25g of dodecanol and 250mL of toluene into a 500mL flask, heat to reflux for 3 hours, cool and dry for later use. Take another 30g of silica gel treated with hydrochloric acid in a 1000mL flask, dry it in vacuum at 150°C for 5 hours, add the above reaction solution under vacuum drive, stir and reflux for 14 hours under the protection of nitrogen, filter, and wash with toluene and methanol in turn to obtain The solid was dried in a vacuum oven at 80° C. for 12 hours to obtain a carbamate chromatographic stationary phase. Elemental analysis: C: 11.8%, N: 0.8%. Infrared spectrum: 2930 and 2859cm -1 Alkyl characteristic absorption peak, 1703cm -1 Carbonyl characteristic absorption peak, 1533cm -1 The characteristic absorption peak of the amide bond. The results of elemental analysis and infrared spectroscopy confirmed that the structure of the stationary phase is:

[0026]

Embodiment 3

[0028] The difference from Example 1 is that stearyl alcohol is used instead of dodecanol. Elemental analysis: C: 16.3%, N: 0.8%. Infrared spectrum: 2930 and 2858cm -1 Alkyl characteristic absorption peak, 1703cm -1 Carbonyl characteristic absorption peak, 1530cm -1 The characteristic absorption peak of the amide bond. The results of elemental analysis and infrared spectroscopy confirmed that the structure of the stationary phase is:

[0029]

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PUM

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Abstract

The invention relates to an efficient liquid phase chromatogram stationary phase which is characterized in that gel in the structure is a particle with hydroxyl, R1 is methyl or ethyl, m is equal to 3-8 and n is equal to 3-29. The liquid phase chromatogram stationary phase has the following advantages: 1, the structure is novel, a polar carbamic acid ester structure is embedded in a hydrophobic carbon chain, wherein an alkyl is at the tail end of an ester bond of the carbamic acid ester (O-alkyl), so that the effect of silicon hydroxyl on the surface of filler on separation can be benefited to being eliminated due to the principle of electrostatic screening, and the compatibility of chromatograph filler and pure water moving phase can be improved; 2, the preparation process for the stationary phase is simple and reliable, and the raw material is easy to obtain, thus being beneficial to batch production of the stationary phase; and 3, the liquid phase chromatogram stationary phase has wide application range. The stationary phase is a pervasive reversed phase chromatography stationary phase, has good analysis property to most polar and nonpolar compound, and has good market application prospect. The invention discloses a preparation method thereof.

Description

technical field [0001] The invention relates to a liquid chromatographic stationary phase and a preparation method thereof, in particular to a novel reversed phase liquid chromatographic stationary phase whose bonded phase is an alkane carbamate. Background technique [0002] Since Kirland first prepared reversed-phase liquid chromatography stationary phase in 1970, reversed-phase high-performance liquid chromatography has been widely used in the separation and purification of chemistry, medicine, food, biology, environment and other fields. According to statistics, about 80% of liquid chromatographic separations are performed in reversed-phase chromatography mode (Qiu H D, Takafuji M, Liu X, et al. Anal. Bioanal. Chem. 2011, 399, 3307-3322; Kirkland J J.J. Chromatogr.A, 2004, 1060, 50-57; Jiang Shengxiang, Liu Xia. Chromatography, 2007, 25, 163-173; Liu Daojie, Deng Aixia. Chemical Reagents, 2004, 26, 10-14). [0003] Compared with coated stationary phases, the ligands on ...

Claims

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Application Information

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IPC IPC(8): B01J20/283B01J20/30
Inventor 郝卫强庄韦陈强孙小丽
Owner CHANGZHOU HIGH TECH RES INST OF NANJING UNIV
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