Bonded silica gel stationary phase with multi-acting-force mixed modes as well as preparation method and application thereof

A bonded silica gel, mixed-mode technology, applied in the field of chromatographic separation, can solve the problems of weak hydrophobicity, lack of aromatic selectivity, weak hydrophobicity, etc., and achieve the effects of low preparation cost, wide application of preparation methods, and high bonding capacity

Inactive Publication Date: 2014-02-05
HENAN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The application of ionic liquids in liquid chromatography stationary phases is mainly due to the imidazolium cation leading to multiple interaction mechanisms between the chromatographic stationary phase and the analyte, such as strong anion exchange, but also weak hydrophobic and electrostatic interactions. At present, the ionic liquid stationary phase has been used to separate polycyclic aromatic hydrocarbons, phenol, aniline, benzoic acid, inorganic anions and other substances, although this new stationary phase has improved the separation selectivity of complex systems to a certain extent, but There are still disadvantages such as weak hydrophobic effect and lack of aromatic selectivity

Method used

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  • Bonded silica gel stationary phase with multi-acting-force mixed modes as well as preparation method and application thereof
  • Bonded silica gel stationary phase with multi-acting-force mixed modes as well as preparation method and application thereof
  • Bonded silica gel stationary phase with multi-acting-force mixed modes as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 4.0 g of chloropropyltriethoxysilyl silica gel into a round bottom flask, add dropwise 1.0 mL of N-octylbenzimidazole and 60 mL of freshly evaporated dry 1,4-dioxane, and reflux at 110°C Stir for 48 h, filter after cooling, and wash the filtered solid with toluene, ethanol-water solution with a ratio of 1:1, water, and methanol three times in sequence, and finally vacuum-dry at 60°C for 8 h to obtain N-octyl Benzimidazole ionic liquid stationary phase. The structure of the stationary phase is:

Embodiment 2

[0040] Add 4.0 g of chloropropyltriethoxysilyl silica gel into a round-bottomed flask, drop into 1.0 mL of N-octadecylbenzimidazole and 60 mL of freshly evaporated dry 1,4-dioxane, at 110°C Reflux and stir for 48 h, filter after cooling, and wash the solid obtained by filtration with toluene, ethanol-water solution with a ratio of 1:1, water, and methanol three times in sequence, and finally vacuum-dry at 60 °C for 8 h to obtain N-octadeca Alkyl benzimidazole ionic liquid stationary phase. The structure of the stationary phase is:

[0041] The stationary phases of Examples 1 and 2 were repeatedly and alternately washed for four months in the range of mobile phase pH=3-9, and the chromatographic column efficiency dropped by about 5%, and the RSD (n=6) of the biphenyl retention time change < 2% , which shows that under the conditions of neutrality, weak acidity and weak alkalinity, the chemical properties of the bonded stationary phase of the present invention are relatively st...

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Abstract

The invention belongs to the technical field of chromatographic separation and particularly relates to a bonded silica gel stationary phase with multi-acting-force mixed modes as well as a preparation method and application thereof. The bonded silica gel stationary phase is an ionic liquid bonded silica gel stationary phase containing aryl and fatty group at the same time. The stationary phase provided by the invention is stable in bonding layer, has separation characteristics of the multi-acting-force multiple modes, and wide application prospect. The preparation method of the bonded silica gel stationary phase is simple, lower in preparation cost and wider in applicable range.

Description

[0001] technical field [0002] The invention belongs to the technical field of chromatographic separation, and in particular relates to a multi-force mixed mode bonded silica gel stationary phase and a preparation method and application thereof. Background technique [0003] Chromatography is the most widely used separation technique today. Its principle is the differential movement of components caused by the difference in force between different components and the stationary phase or mobile phase. Chromatographic stationary phase is the "heart" of chromatographic separation. There are many types of liquid chromatography, including reversed-phase chromatography (RPLC), normal-phase chromatography (NPLC), hydrophobic chromatography (HIC), ion-exchange chromatography (IEC), etc. For these traditional stationary phases, the separation mechanism and mode are single. For example, reversed-phase chromatography C18 stationary phase mainly relies on hydrophobic interaction to sepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/08C07B63/00
Inventor 赵文杰马丽刁小琼郑利梅张书胜
Owner HENAN UNIVERSITY OF TECHNOLOGY
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