A kind of quartz capillary chiral separation column for racemate separation and preparation method thereof

A quartz capillary and chiral separation technology, applied in the field of gas chromatographic separation, can solve the problem that the racemate cannot be separated, and achieve the effect of obvious advantages of chiral separation

Inactive Publication Date: 2017-10-24
YUNNAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still some racemates that cannot be separated well on this type of chiral column, so the development and research of new high-selectivity, stable gas chromatography chiral stationary phase is the research of gas chromatography chiral separation technology. one of the directions

Method used

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  • A kind of quartz capillary chiral separation column for racemate separation and preparation method thereof
  • A kind of quartz capillary chiral separation column for racemate separation and preparation method thereof
  • A kind of quartz capillary chiral separation column for racemate separation and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) synthetic porous organic material CC10 is used as the chiral stationary phase of the chromatographic column of the present invention (as figure 1 shown), the specific process is as follows:

[0017] Add 0.6g of (1R,2R)-1,2-bis(4-fluorophenyl)-1,2-ethylenediamine dihydrochloride into 40mL of deionized water and ultrasonically dissolve it, then add 0.54mL of triethyl The amine was basified to become free diamine, then 15 mL of dichloromethane was added for shaking, and the mixture was allowed to stand to separate layers. The liquid was separated, and the organic layer was vacuum-dried at 100° C. to obtain 0.36 g of (1R,2R)-1,2-bis(4-fluorophenyl)-1,2-ethylenediamine.

[0018] Dissolve 0.36 g of the prepared (1R,2R)-1,2-bis(4-fluorophenyl)-1,2-ethylenediamine and 0.16 g of 1,3,5-trimesaldehyde in 10 mL of dry 0.25 g of molecular sieves and 8 μL of trifluoroacetic acid were added, and the reaction solution was sealed and stirred at room temperature for 96 hours. Then...

Embodiment 2

[0022] The quartz capillary chiral separation column prepared in Example 1 is used to resolve many racemates including alcohols, esters, ethers, epoxy compounds, halogenated hydrocarbons, organic acids, etc., some typical resolutions See the chromatogram figure 2 .

[0023] Depend on figure 2 It can be seen that the chromatographic column of the present invention has better chiral resolution performance for the above-mentioned racemate.

Embodiment 3

[0025] Use the quartz capillary chiral separation column prepared in Example 1 and the commercial β-DEX 120 capillary chiral separation column to resolve some racemates and compare their chiral resolution effects. The comparative resolution chromatograms See image 3 .

[0026] image 3 The first column and the third column are the resolution chromatograms of some racemates on the chromatographic column of the present invention; the second column and the fourth column are the chiral separation of the same racemate in commercial β-DEX 120 capillaries Split chromatogram on column.

[0027] Depend on image 3 It can be seen that these tested racemates are not resolved on the commercial β-DEX 120 capillary chiral separation column, but the chromatographic column of the present invention can better resolve these racemates. Therefore, compared with the commercial β-DEX120 capillary chiral separation column, the chromatographic column of the present invention has obvious chiral r...

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Abstract

The invention discloses a quartz capillary chiral separation column used for the separation of racemates and a preparation method thereof. First, the chiral porous material CC10 was synthesized as the stationary phase. Take the quartz capillary column and fill it with sodium hydroxide solution for 2 hours to roughen its inner wall, then sequentially rinse with deionized water, rinse with hydrochloric acid, rinse with deionized water, and pass dry nitrogen. Get the synthesized chiral stationary phase CC10 and dissolve it in dichloromethane to prepare a solution, then mix it with the dichloromethane solution of OV-1701, and fill this mixed solution into the above-mentioned treated quartz capillary column using static The desired capillary chiral separation column was prepared by the method of column preparation. The chromatographic separation column exhibits excellent chiral resolution performance for many racemates including alcohols, esters, ethers, epoxy compounds, halogenated hydrocarbons, organic acids, etc.

Description

technical field [0001] The invention relates to a gas chromatographic quartz capillary separation column, in particular to a quartz capillary gas chromatographic chiral separation column suitable for racemate separation, and belongs to the technical field of gas chromatographic separation. Background technique [0002] Chirality is one of the basic properties of substances in nature. Amino acids, proteins, nucleic acids, sugars, etc. that make up living organisms all have chirality. Many drugs currently in use also have chirality. However, in racemic drugs, only one enantiomer is often effective, while its mirror image molecule is not only ineffective, but sometimes partially offsets the highly active isomer. Drug effects in the body, or produce toxic metabolites or cause serious side effects. In addition to drugs, some insecticides, plant growth regulators, herbicides, spices, etc. also have chirality, and the enantiomers of their molecules often show different biological...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): B01J20/29C07B57/00C07C27/26C07C29/76C07C31/125C07C33/03C07C41/36C07C43/04C07C51/47C07C53/126C07C17/389C07C19/01C07C67/56C07C69/14C07C69/63C07D301/32C07D303/04
Inventor袁黎明章俊辉
OwnerYUNNAN NORMAL UNIV