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Preparation method of quaternary ammonium base component in corydalis tuber extract

The technology of extract and Corydalis Corydalis, which is applied in the field of preparation of quaternary ammonium base components in Corydalis Corydalis extract, achieves the effects of mild reaction conditions, high reaction conversion efficiency and easy operation.

Inactive Publication Date: 2020-04-24
TAIZHOU GUOKEHUAWU BIOMEDICAL TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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  • Preparation method of quaternary ammonium base component in corydalis tuber extract
  • Preparation method of quaternary ammonium base component in corydalis tuber extract
  • Preparation method of quaternary ammonium base component in corydalis tuber extract

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Embodiment 1

[0025] Add 5.0 g of Corydalis extract to a 250 ml reaction bottle, add 100 ml of ethanol, stir for 0.5 h, add 0.3 g of potassium acetate, stir for 10 min, add 0.3 g of I 2 20 ml ethanol solution, stirred at room temperature for 1 h. After the reaction was detected by HPLC, it was concentrated to remove the solvent, diluted with water, filtered with suction, and washed with a large amount of water. The resulting solid product was dried under vacuum to obtain 0.05 g of a brownish-yellow solid, analyzed by HPLC, wherein the quaternary ammonium base content was 55.2% based on dehydrocorydaline, see figure 2 , the comparative spectrum of the sample solution before and after the reaction is as follows image 3 As shown, two main tertiary amine bases in the extract—the peaks of tetrahydropalmatine and first element disappeared in the reaction solution, and the peaks of palmatine and dehydrocorydalline increased significantly, and the tertiary amine bases in the extract were almost ...

Embodiment 2

[0027] Add 5.0 g of Corydalis extract to a 250 ml reaction bottle, add 100 ml of methanol, stir for 0.5 h, add 0.3 g of sodium acetate, stir for 10 min, add 0.2 g of I 2 20 ml methanol solution, stirred at room temperature for 0.5 h. After the reaction was detected by HPLC, it was concentrated to remove the solvent, diluted with water, filtered with suction, and washed with a large amount of water. The resulting solid product was dried under vacuum to obtain 0.04 g of a tan solid. Through HPLC analysis, wherein the content of quaternary ammonium base is 58.5% in terms of dehydrocorydaline.

Embodiment 3

[0029] Add 5.0 g of Corydalis extract to a 250 ml reaction bottle, add 100 ml of water, stir for 0.5 h, add 0.3 g of sodium acetate, stir for 10 min, add 0.35 g of I 2 20 ml of aqueous solution, stirred at room temperature for 1.2 h. After the reaction was detected by HPLC, it was concentrated to remove the solvent, diluted with water, filtered with suction, and washed with a large amount of water. The resulting solid product was dried under vacuum to obtain 0.045 g of a tan solid. Through HPLC analysis, wherein the content of quaternary ammonium base is 56.3% in terms of dehydrocorydaline.

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Abstract

The invention provides a preparation method of a quaternary ammonium base component in a corydalis tuber extract. According to the preparation method, protoberberine tertiary amine bases in a corydalis tuber extract are oxidized into berberine quaternary ammonium bases, wherein the two protoberberine tertiary amine bases with the highest content, such as tetrahydropalmatine and corydaline, in corydalis tuber are respectively oxidized into palmatine and dehydrocorydaline; after the reaction is completed, filtering is performed; and the supernatant is concentrated and dried to obtain the corydalis tuber extract component rich in the berberine quaternary ammonium compound, wherein the total alkali content reaches more than 50%. According to the invention, the preparation method is simple in process, efficient, high in recovery rate and low in production cost, and provides a good technical scheme for safe, effective and controllable development of corydalis tuber alkaloid component preparations.

Description

technical field [0001] The invention relates to the field of drug synthesis, in particular to a preparation method of quaternary ammonium base components in Corydalis Corydalis extract. Background technique [0002] Corydalis yanhusuo (Yuanhu) is the tuber of Corydalis yanhusuo W. T. Wang, a plant of the poppy family. It is warm in nature and bitter in taste, can promote blood circulation and disperse blood stasis, benefit qi and relieve pain. It is one of the famous "Eight Flavors of Zhejiang Province" and has high medicinal value. Modern medicinal chemistry and pharmacology experiments have shown that the main active ingredients in Corydalis Corydalis are two types of alkaloids, tertiary amine and quaternary ammonium, of which the content of tertiary amine base is about 0.65%, and the content of quaternary ammonium base is about 0.3% (He Kai, Gao Jianli , Zhao Guangshu. Research progress on chemical constituents, pharmacological effects and quality control of Corydalis Cor...

Claims

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Application Information

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IPC IPC(8): A61K36/66A61K125/00
CPCA61K36/66
Inventor 梁鑫淼赵耀鹏王超然乔健郭秀洁
Owner TAIZHOU GUOKEHUAWU BIOMEDICAL TECH CO LTD
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