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Rapid preparation and application of MBA bridged cyclodextrin functionalized chiral monolithic column

A technology of cyclodextrin and monolithic column, which is applied in the field of analytical chemistry, can solve the problems of cumbersome preparation process, no application of bridging cyclodextrin, and long time consumption, and achieve simple preparation process, improved chiral separation performance, and improved retention Effect

Active Publication Date: 2020-02-14
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 column
  • Rapid preparation and application of MBA bridged cyclodextrin functionalized chiral monolithic column
  • Rapid preparation and application of MBA bridged cyclodextrin functionalized chiral monolithic column

Examples

Experimental program
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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, and then Dry with nitrogen at room temperature and 0.4 MPa for 30 min; in order to introduce amino groups 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 cover both ends with silicon The capillary was sealed with rubber, and the capillary was heated in a water bath at 60 °C for 24 h, rinsed with methanol for 30 min, and then dried with nitrogen at 70 °C and 0.4 MPa for 3 h to obtain a pretreated quartz capillary for use in further use;

[0027](2) Accurately weigh 1 mg MBA, 14.93 mg SH-β-CD, 1 mg AIBA and 20...

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 preparation and application thereof, and belongs to the field of analytical chemistry. According to theMBA bridged cyclodextrin functionalized chiral monolithic column, a cyclodextrin SH-beta-CD and a ligand derivatizing agent MBA are first dissolved in deionized water, a bridged cyclodextrin is formedby a reaction under the condition of AIBA as an initiator, then a nucleophilic reagent urea and a protonation reagent formaldehyde solution are added, and the MBA bridged cyclodextrin functionalizedchiral monolithic column is prepared by one-step polymerization under the action of the catalyst urea. A method for preparing the MBA bridged cyclodextrin functionalized chiral monolithic column is simple, the reaction is fast, a cyclodextrin bimolecular bridged structure constructed through a functional bridge can fully exert the synergistic effect between every two molecules and a bridge chain,the chiral recognition ability of a stationary phase is significantly enhanced, the MBA bridged cyclodextrin functionalized chiral monolithic column is enabled to show excellent resolution ability todifferent types of chiral drugs such as amino acid and metoprolol tartrate in electrochromatography, and thus the MBA bridged cyclodextrin functionalized chiral monolithic column can be used in the field of chiral resolution of the 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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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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