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Method for extracting protopine from japanese hylomecon rhizome

A technology for proto-opioid and jujube seven, which is applied in the field of natural product extraction, can solve the problems of no extraction, separation and identification of alkaloid components, little research on chemical components of jujube seven, and the like, and the method is simple and easy to implement and low in cost. Effect

Inactive Publication Date: 2013-08-28
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, there are very few studies on the chemical constituents of Jujube seven at home and abroad, and there are no reports on the extraction, separation and identification of its alkaloid constituents

Method used

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  • Method for extracting protopine from japanese hylomecon rhizome
  • Method for extracting protopine from japanese hylomecon rhizome
  • Method for extracting protopine from japanese hylomecon rhizome

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The method for extracting the original opioid from Jujube seven, comprises the following steps:

[0029] 1) Take about 7.0kg of Jujube seven coarse powder, reflux extraction with 95% ethanol for 3 times, each time for 2 hours, recover the extract, concentrate under reduced pressure to obtain the extract, use 15L of the extract for 1.0kg, the mass concentration is 2% After dissolving the hydrochloric acid, filter it, pass the filtrate through the C008 type cation exchange resin according to the flow rate of 1BV / h, wash the resin with deionized water until it is neutral, and then use 13L of ammonia water with a mass concentration of 10% to alkalize the resin. The resin was soaked and extracted with ethyl acetate and filtered, and the solvent was recovered under reduced pressure to obtain 31.0 g of the total alkaloids of Jujube chinensis;

[0030] 2) Chromatography of 31.0 g of the total alkaloids of Jujube seven on alkaline silica gel column at normal pressure, with chlor...

Embodiment 2

[0042] The method for extracting the original opioid from Jujube seven, comprises the following steps:

[0043]1) Take about 7.0kg of the coarse powder of Jujube seven, extract twice with 95% ethanol under reflux, each time for 3 hours, recover the extract, concentrate under reduced pressure to obtain the extract, and use 12L of hydrochloric acid with a mass concentration of 2% for 1.0kg of the extract After dissolving, filter, pass the filtrate through the C008 type cation exchange resin according to the flow rate of 1.2BV / h, wash the resin with deionized water until it is neutral, and then use 12L of ammonia water with a mass concentration of 4% to alkalize the resin. The resin was soaked and extracted with ethyl acetate and then filtered, and the solvent was recovered under reduced pressure to obtain 32.2 g of total alkaloids of Jujube chinensis;

[0044] 2) Put 32.2g of the total alkaloids of jujube seven through normal pressure alkaline silica gel column chromatography, u...

Embodiment 3

[0048] The method for extracting the original opioid from Jujube seven, comprises the following steps:

[0049] 1) Extract about 7.0kg of the coarse powder of Jujube seven with 95% ethanol under reflux for 4 times, each time for 2 hours, recover the extract, concentrate under reduced pressure to obtain the extract, and use 18L of hydrochloric acid with a mass concentration of 1% for 1.0kg of the extract After dissolving, filter, pass the filtrate through the C008 type cation exchange resin according to the flow rate of 1.5BV / h, wash the resin with deionized water to neutrality, and then use 13L of ammonia water with a mass concentration of 15% to alkalize the resin, and the alkalized The resin was soaked and extracted with ethyl acetate, and the solvent was recovered under reduced pressure to obtain 32.8 g of the total alkaloids of Jujube chinensis;

[0050] 2) Chromatography of 32.8g of total alkaloids of Jujube seven on alkaline silica gel column under normal pressure, with ...

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Abstract

The present invention discloses a method for extracting protopine from japanese hylomecon rhizome, and belongs to the technical field of natural product extraction. The method comprises the following steps: 1) taking japanese hylomecon rhizome total alkaloid extract, adding to an alkaline silica gel column, adopting a chloroform-methanol system as an eluent to carry out gradient elution, mixing distillates, and evaporating the solvent to obtain a first collected part; 2) taking the first collected part, adding to the alkaline silica gel column, adopting a chloroform-methanol system as an eluent to carry out gradient elution, mixing distillates having the same main fleck, and evaporating the solvent to obtain a second collected part; 3) taking the second collected part, adding to a sephadex column, adopting a chloroform-methanol system as an eluent to carry out isocratic elution, mixing distillates having the same main fleck, and evaporating the solvent to obtain a third collected part; and 4) repeatedly washing the third collected part by using methanol to obtain the protopine. The method has characteristics of simple operation, low cost and high extraction efficiency, wherein the extracted protopine purity is more than 99%.

Description

technical field [0001] The invention belongs to the technical field of natural product extraction, and in particular relates to a method for extracting pro-opiate from Jujube seven. Background technique [0002] Guziqiqi is the root and rhizome of Helianthus chinensis, also known as Heqinghua and Dayeshuqi. It has the effects of dispelling wind and dampness, relaxing tendons and activating collaterals, dissipating blood stasis and reducing swelling, stopping bleeding and relieving pain; it is commonly used by Shaanxi folks It treats rheumatoid arthritis, bruises and other diseases. So far, there are few studies on the chemical constituents of Jujube seven at home and abroad, and there are no reports on the extraction, separation and identification of its alkaloid constituents. [0003] The main alkaloid components in Jujube seven are protopine, cryptopine, coptisine, berberine, sanguinarine, chelerythrine, gold papaverine and so on. Protopine is also known as Protopine, Ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/153
Inventor 郭增军韩燕霞席可李梦怡戴柳江张卉
Owner XI AN JIAOTONG UNIV
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