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Preparation method and application of a polar bridged cyclodextrin chiral monolithic column

A technology of cyclodextrin and monolithic column, which is applied in the field of analytical chemistry to achieve the effects of improved retention, high polarity, and improved chiral separation performance

Active Publication Date: 2021-08-31
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 a polar bridged cyclodextrin chiral monolithic column
  • Preparation method and application of a polar bridged cyclodextrin chiral monolithic column
  • Preparation method and application of a polar bridged cyclodextrin chiral monolithic column

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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 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; after the reaction was completed, the prepared monolithic column was taken out, connected to a liquid chromatography solvent ...

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 firstly dissolving cyclodextrin and N,N-(1,2-dihydroxyethylene) diacrylamide DAA in deionized water, and reacting under the condition of initiator AIBA to form a polar bridged cyclodextrin A polar bridged cyclodextrin chiral monolithic column was rapidly prepared within 30 min by adding urea and formaldehyde through a one-pot thermal polycondensation method. In the present invention, the preparation method is simple and the reaction is fast. By using a highly polar bridging agent to construct a cyclodextrin bimolecular bridge structure, additional hydrophilic interactions can be provided, and the chiral recognition ability of the stationary phase can be significantly enhanced. Chromatography has demonstrated excellent resolution capabilities for various types of drugs such as amino acids and RS-(+)-(4-methoxyphenyl)ethylamine, and can be used as a chromatographic chiral stationary phase 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 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 Patents(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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