Preparation method and application of polar bridging cyclodextrin chiral monolithic column

A cyclodextrin, monolithic column technology, applied in the field of analytical chemistry

Active Publication Date: 2020-10-23
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far, there has been no report on the effect of the type of bridging agent on the chiral separation performance of the bridged cyclodextrin monolithic column. The effect of chiral separation performance is an interesting study

Method used

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  • Preparation method and application of polar bridging cyclodextrin chiral monolithic column
  • Preparation method and application of polar bridging cyclodextrin chiral monolithic column
  • Preparation method and application of polar bridging cyclodextrin chiral monolithic column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A preparation method of a polar bridged cyclodextrin chiral monolithic column, the specific steps are:

[0034] (1) Accurately weigh 0.63 mg DAA, 14.93 mg SH-β-CD, 1 mg AIBA and 200 mg deionized water into a centrifuge tube, vortex at room temperature for 20 minutes, and ultrasonically degas for 20 minutes to form homogeneous solution, and then placed in a water bath at 60 °C for 6 h to obtain a DAA bridged cyclodextrin aqueous solution (characterized as figure 2 , 3 );

[0035](2) Add 100 mg of catalyst and 200 mg of urea to the solution obtained in step (1), vortex at room temperature for 20 min, add 600 mg of formaldehyde solution, vortex for 1 min, and inject rapidly at room temperature with aminopropyl In a quartz capillary column pretreated with trimethoxysilane, both ends were sealed and immersed in a 75 °C water bath for continuous reaction for 30 min; The reacted material was allowed to obtain column C until the pressure stabilized.

Embodiment 2

[0037] Step (1) deionized water is 250 mg, step (2) urea is 250 mg and formaldehyde solution is 500 mg, and other steps are as in Example 1 to obtain column A.

Embodiment 3

[0039] In step (1) deionized water is 225 mg, in step (2) urea is 225 mg and formaldehyde solution is 450 mg, other steps are as in Example 1, and column B can be obtained.

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Abstract

The invention discloses a preparation method and application of a polar bridging cyclodextrin chiral monolithic column, and belongs to the field of analytical chemistry. The monolithic column is prepared by the following steps: dissolving cyclodextrin with N, N-(1, 2-dihydroxyethylene) diacrylamide DAA in deionized water, reacting under the condition of an initiator AIBA to generate polar bridgingcyclodextrin, adding urea and formaldehyde, and quickly preparing the polar bridging cyclodextrin chiral monolithic column within 30 minutes by virtue of a one-pot thermal polycondensation method. The preparation method is simple and rapid in reaction, a cyclodextrin bimolecular bridging structure is constructed by adopting a bridging agent with high polarity; the additional hydrophilic interaction can be provided, the chiral recognition ability of the stationary phase can be significantly enhanced, the excellent resolution ability on a variety of amino acids, RS-(+)-(4-methoxybenzene) ethylamine and other different types of drugs can be displayed in the electrochromatography, and the method can be used as the chromatographic chiral fixation so as to be correspondingly used in the field of drug chiral resolution.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a preparation method and application of a polar bridged cyclodextrin chiral monolithic column. Background technique [0002] In recent years, due to the advantages of high permeability, fast mass transfer and easy preparation of monolithic columns, especially chiral monolithic columns, they have shown extremely high separation potential in the field of chiral separation. Cyclodextrin (CD) is one of the most widely used and economical chiral selectors in the fields of chromatography and electrophoresis. CD is a non-reducing natural oligosaccharide with a unique hydrophobic cavity, which endows CD with the special ability to establish a variety of interactions with analytes to promote chiral recognition, thus making it widely used in the field of chiral monolithic columns . Although a lot of research and significant progress have been made on cyclodextrin chiral mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06B01J20/29B01J20/24B01D15/38
CPCB01D15/3833B01J20/24B01J20/29G01N30/06
Inventor 吕海霞孙浩冉刘玥
Owner FUZHOU UNIV
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