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A kind of classification preparation method of tertiary amine base and quaternary ammonium base in Corydalis extract

The technology of extract and tertiary amine base is applied in the field of preparation of traditional Chinese medicine alkaloid components, which can solve problems such as classification and preparation, and achieve the effects of facilitating quality control, simple process and high purity

Active Publication Date: 2017-03-22
中科榆林能源技术运营有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, although there is a great demand for the preparations of effective parts of Corydalis alkaloids, they are mainly extract tablets or refined total alkaloids through acid extraction, alkali precipitation, and ion exchange resins. Ingredients are sorted by method of preparation

Method used

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  • A kind of classification preparation method of tertiary amine base and quaternary ammonium base in Corydalis extract
  • A kind of classification preparation method of tertiary amine base and quaternary ammonium base in Corydalis extract

Examples

Experimental program
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Effect test

Embodiment 1

[0015] Take 200 mg of the methanol extract of Corydalis Corydalis made from vinegar and dissolve it in 10 mL of 5% methanol water to obtain a 20 mg / mL extract solution. 10g of C18 / WCX filler (particle size 40μm) was filled in an open SPE column tube, first activated with 30mL of methanol, then equilibrated with 30mL of water, and set aside. Pour 10mL of sample into the empty tube above the SPE column, and load the sample onto the SPE column at a speed of about 2mL / min. After the sample is loaded, rinse it with 60mL of 10% methanol water to remove the more polar impurities; then Use 60mL of 80% methanol to elute the tertiary amine alkaloid in two tubes; then wash with pure methanol until the eluate is colorless, and remove other non-alkaloid components with weak polarity; finally, use 1% formic acid The quaternary ammonium alkaloids were eluted with methanol until the eluent was colorless (about 20 mL). After elution, the SPE column returns to white, and after equilibrating wi...

Embodiment 2

[0017] Take 200 mg of the methanol extract of Corydalis Corydalis made from vinegar and dissolve it in 10 mL of 5% methanol water to obtain a 20 mg / mL extract solution. 10g of C18 / WCX filler (particle size 40μm) was filled in an open SPE column tube, first activated with 30mL of ethanol, then equilibrated with 30mL of water, and set aside. Pour 10mL of sample into the empty tube above the SPE column, and load the sample onto the filler at a speed of about 2mL / min. After the sample is loaded, rinse it with 60mL of 5% ethanol water to remove the more polar impurities; then use Divide 60mL of 50% ethanol into two tubes to elute tertiary amine alkaloids; then wash with pure ethanol until the eluate is colorless, and remove other non-alkaloid components with weak polarity; finally, use 80% acetic acid containing 80 % ethanol to elute the quaternary ammonium alkaloid until the eluent is colorless (about 50 mL). After elution, the SPE column returns to white, and after equilibrating...

Embodiment 3

[0019] Take 200mg of the 80% ethanol extract of Corydalis made of vinegar and dissolve it in 10mL of water to obtain a 20mg / mL extract solution. 10g of C18 / WCX filler (particle size 40μm) was filled in an open SPE column tube, first activated with 30mL of ethanol, then equilibrated with 30mL of water, and set aside. Pour 10mL of sample into the empty tube above the SPE column, and load the sample onto the filler at a speed of about 2mL / min. After the sample is loaded, rinse it with 60mL of 5% ethanol water to remove the more polar impurities; then use Divide 60mL of 50% ethanol into two tubes to elute tertiary amine alkaloids; then wash with pure ethanol until the eluate is colorless, and remove other non-alkaloid components with weak polarity; finally, use 80% acetic acid containing 80 % ethanol to elute the quaternary ammonium alkaloid until the eluent is colorless (about 50 mL). After elution, the SPE column returns to white, and after equilibrating with water, the sample ...

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Abstract

The invention provides a method for classifying and preparing tertiary amine alkaloid and quaternary ammonium alkaloid from corydalis extract. The method comprises the following steps of eluting different solvents according to a like component preparation method by adopting a C18 / WCX (Weak cation exchange) type separating material with the combination of the hydrophobic effect and a weak cation exchange function, removing impurities, and enriching tertiary amine alkaloid and quaternary ammonium alkaloid, which are completely different in functional activity, contained in the corydalis extract respectively, wherein the total alkali contents in two like components can reach more than 65% and more than 90% respectively through HPLC (High Performance Liquid Chromatography) analysis. The preparation method has simple process, and has high efficiency and high recovery rate, the used separating material can be used repeatedly, the production cost is low, and the method can provide a good technical scheme for developing safe, efficient and controllable Chinese herbal preparations with alkaloids components.

Description

[0001] Technical field: [0002] The invention belongs to the technical field of separation and purification of alkaloids, and in particular relates to a method for preparing traditional Chinese medicine alkaloid components. [0003] Background technique: [0004] 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" and has high medicinal value. Modern medicinal chemistry and pharmacology experiments have shown that the main active ingredients in 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. Corydalis chemical constituents, pharmacological effects and quality control re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/42C07G5/00
Inventor 梁鑫淼王超然郭秀洁张秀莉郭志谋薛兴亚
Owner 中科榆林能源技术运营有限责任公司
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