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Method for separating anisodamine and/or tropic acid mixed enantiomer

A technology of anisodamine and tropic acid, applied in the analysis of materials, material analysis by electromagnetic means, measuring devices, etc., can solve the problems of inability to separate the six isomers, and achieve the effect of rapid separation and fast separation speed

Inactive Publication Date: 2018-05-04
BEIJING UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] According to the separation method of the prior art, the 6 isomers of the mixture of anisodamine and tropic acid cannot be effectively separated

Method used

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  • Method for separating anisodamine and/or tropic acid mixed enantiomer
  • Method for separating anisodamine and/or tropic acid mixed enantiomer
  • Method for separating anisodamine and/or tropic acid mixed enantiomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Selection of Cyclodextrin Derivatives

[0074] Take sulfonated-β-dextrin polymer, hydroxypropyl-β-cyclodextrin (HP-β-CD), methylated-β-cyclodextrin (Me-β-CD), sulfobutyl- β-cyclodextrin (SE-β-CD), mixture of SE-β-CD and Me-β-CD, mixture of SE-β-CD and HP-β-CD, SE-β-CD and sulfonated- A mixture of β-dextrin polymers was used as a resolving agent to resolve anisodamine and tropic acid.

[0075] The concentration of the resolving agent SE-β-CD in the electrophoresis buffer is 10mg / mL, the pH of the electrophoresis buffer is 3, the temperature is room temperature, the voltage is -15kV, and the gravity injection is 5s. The result is as follows: figure 1 shown. figure 1 The peaks in the figure are from left to right, peaks 1, 2, 4, and 5 are enantiomers of anisodamine. Peaks 3 and 6 are enantiomers of tropic acid.

[0076] The concentration of the resolving agent SE-β-CD and Me-β-CD in the electrophoresis buffer is 10mg / mL, the pH of the electrophoresis buffer is 4, the t...

Embodiment 2

[0084] Effect of buffer pH value on the separation degree of anisodamine and tropic acid

[0085] The influence of the chiral separation when the pH value changed from 2.0 to 9.0 was investigated. The concentration of SE-β-CD in the electrophoresis buffer is 10mg / mL, the temperature is room temperature, and the voltage is -15kV. The capillary electrophoresis diagrams when the pH of the electrophoresis buffer is 2, 2.5, 3, 4 and 5 are as follows Figure 8 shown. The capillary electrophoresis picture when the pH of the electrophoresis buffer is 6 is as follows: Figure 9 shown. The capillary electrophoresis images when the pH of the electrophoresis buffer is 7, 8 and 9 are as follows Figure 10 shown. In the experiment, it was found that when the pH was 2.0-5.0, due to the small electroosmotic flow, the sample could not be driven to migrate to the negative electrode, so the sample peak could not be detected under the positive voltage. Using reverse voltage in the range of pH...

Embodiment 3

[0087] Effect of SE-β-CD Concentration on the Resolution of Anisodamine and Tropic Acid

[0088] In the experiment, the change of the separation degree of anisodamine and tropic acid samples was investigated when the temperature was room temperature, the pH was 3.0, the voltage was -15kV operating voltage, and the concentration of SE-β-CD was 2.5-15mg / mL. The result is as Figure 11 shown. Within the selected range, anisodamine and tropic acid can be separated to varying degrees. When the concentration of SE-β-CD is 2.5 mg / mL, three enantiomers can be separated; the concentration of SE-β-CD is 5-7.5 mg / mL, 4 enantiomers were separated, but the chromatographic peaks between the 3rd enantiomer and the 4th enantiomer overlapped; when the concentration of SE-β-CD was 10mg / mL, anisodamine and The resolution of tropic acid was the best, and the four enantiomers were completely resolved; when the concentration of SE-β-CD was 11.5 mg / mL, the four enantiomers of anisodamine could be ...

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Abstract

The invention discloses a method for separating anisodamine and / or tropic acid mixed enantiomer. The method has the advantages that the anisodamine and tropic acid enantiomers can be respectively separated from a racemization anisodamine and tropic acid mixture; the structural formula is shown in formulas I to VI; the formulas I to VI are shown in the description. The method is a capillary electrophoresis method, and comprises the following steps that (1) an electrophoresis buffer solution contains a chiral resolution agent, and the chiral resolution agent is selected from a mixture of sulfobutyl-beta-cyclodextrin, and / or sulfobutyl-beta-cyclodextrin and hydroxypropyl-beta-cyclodextrin; (2) the separation voltage is -8kV to -18kV.

Description

technical field [0001] The present application relates to a separation method of anisodamine and / or tropic acid mixed enantiomers and the separated enantiomers. Background technique [0002] Anisodamine is an alkaloid isolated from the Solanaceae plant Anisodamine tangutum in my country, and has two chiral centers. It has smooth muscle relaxation, relieves vasospasm and thus has analgesic effect, and there are tablets and injections in ready-made medicine. Injections are often used clinically, and can be used to treat infectious toxic shock, sciatica, gastric and duodenal ulcers, retinitis pigmentosa and other diseases. Tropic acid is a synthetic intermediate of various chiral drugs, with one chiral center. It has certain toxicity and mutagenic effects. Tropic acid is also one of the degradation products of anisodamine. The aqueous solution of anisodamine is easily degraded into tropic acid, and the content of tropic acid increases continuously within a certain period of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/447
CPCG01N27/447
Inventor 袁瑞娟王雄飞孙毅坤詹雪艳孙科
Owner BEIJING UNIV OF CHINESE MEDICINE
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