Eureka AIR delivers breakthrough ideas for toughest innovation challenges, trusted by R&D personnel around the world.

Preparation method and applications of alkylimidazole type ion liquid functionalized quinine silica gel chromatography stationary phase

An alkylimidazole-type, ionic liquid technology, applied in the field of chromatographic stationary phase, to achieve the effect of easy-to-obtain raw materials in the preparation process, novel stationary phase structure, and realize the effect of commercial batch production

Active Publication Date: 2019-11-05
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
View PDF4 Cites 10 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, there are no reports on quinine-bonded silica gel chromatography stationary phases functionalized with alkylimidazole-type ionic liquids

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method and applications of alkylimidazole type ion liquid functionalized quinine silica gel chromatography stationary phase
  • Preparation method and applications of alkylimidazole type ion liquid functionalized quinine silica gel chromatography stationary phase
  • Preparation method and applications of alkylimidazole type ion liquid functionalized quinine silica gel chromatography stationary phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] (1) Ultrasonically disperse 3.0 g of 3-mercaptopropyltriethoxysilane coupling agent and 3.0 g of silica gel in 30.0 ml of dimethylbenzene solvent, and raise the temperature to 90°C under the protection of nitrogen or argon for mechanical stirring reaction After 48 h, cool to room temperature, wash by centrifugation, and dry in vacuum to obtain mercaptopropyl silica gel;

[0062] (2) Ultrasonic disperse 2.8 g of mercaptopropyl silica gel, 2.0 g of quinine, and 28.0 mg of azobisisobutyronitrile in 20.0 ml of anhydrous chloroform (add molecular sieve to remove water), heat up to 65°C and mechanically stir and reflux the reaction After 30 hours, after the mixture was cooled to room temperature, it was centrifuged and washed, and dried in vacuum to obtain polyquinine silica gel;

[0063] (3) Add 2.1 ml of 2-chloroethyl isocyanate dropwise to 31.0 ml of anhydrous dichloromethane homogeneous dispersion containing 2.6 g of polyquinine silica gel, mechanically stir at room tempe...

Embodiment 2

[0067] (1) Ultrasonically disperse 2.5 g of 3-mercaptopropyltrimethoxysilane coupling agent and 3.0 g of silica gel in 42.0 ml of benzene solvent, raise the temperature to 100°C under the protection of nitrogen or argon atmosphere, and react with mechanical stirring for 20 h. Cool to room temperature, wash by centrifugation, and dry in vacuum to obtain mercaptopropyl silica gel;

[0068] (2) Ultrasonic disperse 2.8 g of mercaptopropyl silica gel, 2.8 g of quinine and 50.0 mg of azobisisobutyronitrile in 22.0 ml of anhydrous chloroform (add molecular sieve to remove water), heat up to 100°C and mechanically stir and reflux the reaction After 22 h, the mixture was cooled to room temperature, washed by centrifugation, and dried in vacuum to obtain polyquinine silica gel;

[0069] (3) Add 1.5 ml of chloroethyl isocyanate dropwise to 20.0 ml of anhydrous chloroform homogeneous dispersion containing 2.6 g of polyquinine silica gel, and react with mechanical stirring at room temperat...

Embodiment 3

[0073] (1) Ultrasonically disperse 3.5 g of 3-mercaptopropyltriethoxysilane coupling agent and 3.0 g of silica gel in 28.0 ml of toluene solvent, raise the temperature to 90°C under the protection of nitrogen atmosphere, and react with mechanical stirring for 36 h, then cool to room temperature, centrifugal washing, and vacuum drying to obtain mercaptopropyl silica gel;

[0074] (2) Ultrasonic disperse 2.8 g of mercaptopropyl silica gel, 2.5 g of quinine and 30.0 mg of azobisisobutyronitrile in 15.0 ml of anhydrous chloroform, heat up to 70°C and mechanically stir and reflux for 30 hours, and wait for the mixture to cool to After room temperature, centrifuge and wash, and vacuum dry to obtain polyquinine silica gel;

[0075] (3) Add 1.8 ml of 3-chloropropyl isocyanate dropwise to 25.0 ml of anhydrous chloroform homogeneous dispersion containing 2.6 g of polyquinine silica gel, mechanically stir at room temperature and react for 22 h, centrifuge, wash, and vacuum dry. Obtain p...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
wavelengthaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation method of an alkylimidazole type ion liquid functionalized quinine silica gel chromatography stationary phase. The preparation method comprises: carrying out a reaction on a silane coupling agent and a silica gel matrix in an alkylbenzene solvent to obtain a mercaptopropyl silica gel; carrying out a reaction on the mercaptopropyl silica gel, quinine and azobisisobutyronitrile in an organic solvent, wherein the quinine is polymerized on the surface of the mercaptopropyl silica gel through a surface radical chain transfer reaction to obtain a polyquinine silica gel; and modifying the surface of the polyquinine silica gel with an alkylimidazole type ion liquid through a nucleophilic substitution reaction in an organic solvent by using halogenated isocyanate as a bridging molecule to prepare the alkylimidazole type ion liquid functionalized quinine silica gel chromatography stationary phase. According to the present invention, the chromatographic separation and selection performance results show that the prepared alkylimidazole type ion liquid functionalized quinine silica gel chromatography stationary phase can achieve the baseline separation of sulfonamides and base nucleosides in a hydrophilic interaction mode, and can further achieve the separation of non-polar compounds and chiral compounds in a reverse phase mode.

Description

technical field [0001] The invention relates to a preparation method of a liquid chromatography stationary phase, in particular to a silica gel chromatography stationary phase whose bonded phase is an alkylimidazole-type ionic liquid functionalized quinine, and belongs to the technical field of chromatography stationary phases. Background technique [0002] High performance liquid chromatography (HPLC) plays an important role in the field of separation and analysis. Stationary phase is the heart of chromatographic separation technology. The development of chromatographic technology is closely related to the innovation of chromatographic stationary phase. development is of great significance. [0003] As a natural plant alkaloid, quinine has cheap and easy-to-obtain raw materials; it contains benzopyridine, tertiary amine positive center, multiple chiral sites, and easy-to-modify hydroxyl and terminal olefin functional groups, which are suitable for modifying small molecular ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/30
CPCB01D15/305B01J20/286
Inventor 邱洪灯周行陈佳
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com