Rapid preparation and application of mba-bridged cyclodextrin-functionalized chiral monolithic columns

A cyclodextrin and monolithic column technology, applied in the field of analytical chemistry, can solve the problems of cumbersome preparation process, no application of bridged cyclodextrins, long time consumption, etc., and achieves simple preparation process, improved chiral separation performance, and improved retention. Effect

Active Publication Date: 2021-09-28
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, there are few developments for bridged cyclodextrin, especially in the application of enantiomer separation. In addition, the preparation process of BCD is cumbersome and time-consuming, and there is no application of bridged cyclodextrin monolithic column.

Method used

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  • Rapid preparation and application of mba-bridged cyclodextrin-functionalized chiral monolithic columns
  • Rapid preparation and application of mba-bridged cyclodextrin-functionalized chiral monolithic columns
  • Rapid preparation and application of mba-bridged cyclodextrin-functionalized chiral monolithic columns

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 The preparation method of MBA-bridged cyclodextrin functionalized chiral monolithic column, the specific steps are:

[0026] (1) Wash the fused silica capillary with 0.1 mol / L HCl solution for 30 min, double distilled water for 30 min, 0.1 mol / L NaOH solution for 4 h, double distilled water for 30 min, methanol for 30 min, Then dry with nitrogen at room temperature and 0.4 MPa for 30 min; in order to introduce the amino group into the inner surface of the capillary to bond the substrate, then fill the capillary with a methanol solution of aminopropyltrimethoxysilane with a volume concentration of 50%, and use Seal the capillary with silicone rubber, heat the capillary in a water bath at 60 °C for 24 h, rinse the capillary with methanol for 30 min, and then dry it with nitrogen at 70 °C and 0.4 MPa for 3 h to obtain a pretreated quartz capillary. for further use;

[0027](2) Accurately weigh 1 mg MBA, 14.93 mg SH-β-CD, 1 mg AIBA and 200 mg deionized water into...

Embodiment 2

[0030] Replace the amount of deionized water added in step (2) of Example 1 with 250 mg, the amount of urea added in step (3) with 250 mg urea, and the amount of formaldehyde solution added with 500 mg. Other steps are as in Example 1. Column A can be obtained.

Embodiment 3

[0032] Replace the amount of deionized water added in step (2) of Example 1 with 225 mg, the amount of urea added in step (3) with 225 mg urea, and the amount of formaldehyde solution added with 450 mg. Other steps are as in Example 1. Column B can be obtained.

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Abstract

The invention discloses an MBA bridged cyclodextrin functionalized chiral monolithic column and its preparation and application, belonging to the field of analytical chemistry. In the monolithic column, the cyclodextrin SH-β-CD and the ligand derivatizer MBA are dissolved in deionized water, and the bridged cyclodextrin is generated by reacting under the condition of AIBA as the initiator, and then the nucleophile urea is added. And the protonating reagent formaldehyde solution, in the next step of polymerization under the action of catalyst urea. The method for preparing the MBA-bridged cyclodextrin functionalized chiral monolithic column is simple and fast, and the cyclodextrin bimolecular bridging structure constructed by the functional bridge can fully exert the synergistic effect between the bimolecules and the bridge chain, Significantly enhance the chiral recognition ability of the stationary phase, so that it can show excellent resolution ability for different types of chiral drugs such as amino acids and metoprolol tartrate in electrochromatography, so it can be applied in the field of chiral resolution of drugs.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to an MBA-bridged cyclodextrin functionalized chiral monolithic column and a rapid preparation method and application thereof. Background technique [0002] Chiral separation is an effective means to obtain a single enantiomer, which has become a hot and difficult point in the field of medicine. Among many chiral separation techniques, capillary electrochromatography (CEC), as a hybrid method of capillary electrophoresis (CE) and high-performance liquid chromatography (HPLC), has attracted more and more attention in chiral separation. Among them, compared with open-tubular columns and packed columns, monolithic columns, especially chiral monolithic columns, are used as separation media due to their advantages such as easy preparation, high permeability, excellent mechanical stability, and wide pH range tolerance, and have been developed. An effective tool for the ana...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/38B01J20/285B01J20/29B01J20/30
CPCB01D15/3833B01J20/285B01J20/29B01J2220/44B01J2220/4812
Inventor 吕海霞孙浩冉
Owner FUZHOU UNIV
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