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Monodisperse magnetic chiral stationary phase as well as preparation method and application thereof

A monodisperse, stationary phase technology, applied in the field of chromatographic stationary phase, can solve the problem of limited chiral recognition ability of cellulose, and achieve the effect of easy separation, high density, and improved π-π effect.

Active Publication Date: 2021-04-06
BEIFANG UNIV OF NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, underivatized cellulose has limited chiral recognition

Method used

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  • Monodisperse magnetic chiral stationary phase as well as preparation method and application thereof
  • Monodisperse magnetic chiral stationary phase as well as preparation method and application thereof
  • Monodisperse magnetic chiral stationary phase as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The preparation method of monodisperse magnetic chiral stationary phase, concrete steps are as follows:

[0040] (1) Preparation of monodisperse polyglycidyl methacrylate microspheres: get 5 mL of glycidyl methacrylate, 5 mL of trimethylolpropane trimethacrylate, 0.2 g of azobisisobutyronitrile, toluene 6mL and cyclohexanol 6mL are ultrasonically dispersed and dissolved, add 40mL of 0.2% (w / v) sodium lauryl sulfate solution and 20mL of 5% (w / v) polyvinyl alcohol, and emulsify until there are no oil droplets to obtain a mixed solution 1. Put 8 mL of polyglycidyl methacrylate microspheres in a 30°C water bath and stir for 30 minutes, add the mixed solution 1, react and swell at 25°C for 24 hours, pass nitrogen gas for 30 minutes, react at 70°C for 24 hours, and then use toluene It was extracted for 24 hours and dried in vacuum to obtain monodisperse polyglycidyl methacrylate microspheres;

[0041] (2) Preparation of monodisperse magnetic polyglycidyl methacrylate microsp...

Embodiment 2

[0048] The preparation method of monodisperse magnetic chiral stationary phase, concrete steps are as follows:

[0049] (1) Preparation of monodisperse polyglycidyl methacrylate microspheres: get 8 mL of glycidyl methacrylate, 8 mL of trimethylolpropane trimethacrylate, 0.5 g of azobisisobutyronitrile, toluene 8mL and cyclohexanol 8mL are ultrasonically dispersed and dissolved, add 0.2% (w / v) sodium lauryl sulfate solution 60mL and 5% (w / v) polyvinyl alcohol 40mL, emulsify until there is no oil drop, and obtain a mixed solution 1. Put 11 mL of polyglycidyl methacrylate microspheres in a 30°C water bath and stir for 30 minutes, add the mixed solution 1, react and swell at 25°C for 24 hours, pass nitrogen gas for 30 minutes, react at 70°C for 24 hours, and then use toluene It was extracted for 24 hours and dried in vacuum to obtain monodisperse polyglycidyl methacrylate microspheres;

[0050] (2) Preparation of monodisperse magnetic polyglycidyl methacrylate microspheres: 8 g o...

Embodiment 3

[0057] The preparation method of monodisperse magnetic chiral stationary phase, concrete steps are as follows:

[0058] (1) Preparation of monodisperse polyglycidyl methacrylate microspheres: 6.5 mL of glycidyl methacrylate, 7 mL of trimethylolpropane trimethacrylate, and 0.4 g of azobisisobutyronitrile, Toluene 7mL and cyclohexanol 7mL are ultrasonically dispersed and dissolved, add 0.2% (w / v) sodium lauryl sulfate solution 50mL and 5% (w / v) polyvinyl alcohol 30mL, emulsify until there is no oil drop, and obtain a mixture Solution 1, put 10mL of polyglycidyl methacrylate microspheres in a 30°C water bath and stir for 30min, add the mixed solution 1, react and swell at 25°C for 24h, inject nitrogen for 35min, react at 70°C for 24h, and then use toluene Soxhlet extraction for 24 hours and vacuum drying to obtain monodisperse polyglycidyl methacrylate microspheres;

[0059] (2) Preparation of monodisperse magnetic polyglycidyl methacrylate microspheres: get 7 g of monodisperse ...

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Abstract

The invention provides a monodisperse magnetic chiral stationary phase as well as a preparation method and an application thereof, and relates to the technical field of chromatographic stationary phases. The monodisperse magnetic polyglycidyl methacrylate microspheres are used as a matrix, cellulose derivatives are added for reversible addition fragmentation chain transfer polymerization reaction, and the cellulose derivatives are bonded on the surfaces of the microspheres to form a cellulose derivative bonded monodisperse magnetic polyglycidyl methacrylate microsphere stationary phase. The monodisperse magnetic chiral stationary phase is simple and efficient in preparation and controllable in reaction, can be used for high performance liquid chromatography, and can efficiently and quickly complete separation of enantiomers.

Description

technical field [0001] The invention relates to the technical field of chromatographic stationary phases, in particular to a monodisperse magnetic chiral stationary phase and a preparation method and application thereof. Background technique [0002] Chirality is one of the essential properties of nature. Some important biological macromolecules related to life activities, such as proteins, polysaccharides, nucleic acids, and enzymes, all have chiral characteristics. In the field of life science research, various physiologically active substances in organisms, such as hormones, vitamins, etc., their physiological activities are all related to their molecular three-dimensional structure and conformation. Most of the commonly used chemical drugs also have chirality, and their pharmacological effects are realized through strict chiral matching and molecular recognition with macromolecules in the body. Studies have found that many enantiomers have differences in biological acti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/29B01J20/30C08J3/12C08L33/14C08L1/04
CPCB01J20/262B01J20/29C08J3/126C08J2333/14C08J2401/04
Inventor 龚波林李建敏
Owner BEIFANG UNIV OF NATITIES
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