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Preparation method of high-purity 1-deoxynojirimycin

A deoxynojirimycin, high-purity technology, applied in the field of industrial production of high-purity 1-deoxynojirimycin preparation, can solve the problems of inapplicability to industrial production, complex process, low yield, etc., and achieve easy removal and simple process , Operational safety effect

Active Publication Date: 2020-06-12
劲牌持正堂药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above-mentioned technical scheme can obtain 1-deoxynojirimycin with higher purity, it has the defects of complex process, high yield and low cost, and the cation exchange resin used is generally a hydrogen type cation exchange resin, so it is necessary to use a high concentration of 1-deoxynojirimycin The acid liquid activates the cation exchange resin into the hydrogen form, and most of the equipment and pipes in the workshop are not acid-resistant materials, so the hydrogen form of the cation exchange resin is not suitable for industrial production
However, the use of ammonium-type cation exchange resins to enrich 1-deoxynojirimycin, combined with strong base anion-exchange resins and hot solvent beating to purify 1-deoxynojirimycin, to prepare high-purity 1-deoxynojirimycin research has not yet been seen. to report

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take 2.0kg of dried mulberry leaves and crush them, add 10 times the amount of solvent to pure water and mix, reflux and extract at 85°C for 2 hours, filter to obtain the filtrate and filter cake, extract the filter cake for 2 hours under the same conditions, filter and combine Twice the filtrate, the pH of the filtrate was adjusted to 4.8 with hydrochloric acid, the precipitate was centrifuged to remove impurities, and the acidified solution was obtained;

[0027] The column volume of the acidified solution is 2L of 001 × 7 (NH + ) cation exchange resin column, washed with water for 5 times the column volume, then eluted with 0.5mol / L ammonia water for 5 times the column volume, and collected the eluate;

[0028] Concentrate the eluate to a volume of 2L at a pressure of 0.09MPa and a temperature of 65°C, and add 1×2(OH - ) strong base type anion exchange resin, collect the non-adsorbed part, and the non-adsorbed part is concentrated and dried under the condition of 65...

Embodiment 2

[0031] Take 2.0kg of dried mulberry leaves and crush them, add 10 times the amount of solvent to pure water and mix, reflux and extract at 85°C for 2 hours, filter to obtain the filtrate and filter cake, extract the filter cake for 2 hours under the same conditions, filter and combine Twice the filtrate, the pH of the filtrate was adjusted to 4.8 with hydrochloric acid, the precipitate was centrifuged to remove impurities, and the acidified solution was obtained;

[0032] Put the acidified solution on LSI-010 (NH + ) cation exchange resin column, washed with water for 5 times the column volume, then eluted with 0.5mol / L ammonia water for 5 times the column volume, and collected the eluate;

[0033] Concentrate the eluent at a pressure of 0.09MPa and a temperature of 65°C, and 1×2(OH - ) strong base type anion exchange resin, collect the non-adsorbed part, and the non-adsorbed part is concentrated and dried at a pressure of 0.09 MPa and a temperature of 65 ° C to obtain a crud...

Embodiment 3

[0036] Take 2.0kg of dried mulberry leaves and crush them, add 10 times the amount of solvent to pure water and mix, reflux and extract at 85°C for 2 hours, filter to obtain the filtrate and filter cake, extract the filter cake for 2 hours under the same conditions, filter and combine Two filtrates, the filtrate was adjusted to pH 4.2 with malic acid, and the precipitate was centrifuged to remove impurities to obtain an acidified solution;

[0037] The column volume of the acidified solution is 2L of 001 × 8 (NH + ) cation exchange resin column, washed with water for 5 times the column volume, then eluted with 0.5mol / L ammonia water for 5 times the column volume, and collected the eluate;

[0038] Concentrate the eluent at a pressure of 0.09MPa and a temperature of 65°C, and 1×2(OH -) strong base type anion exchange resin, collect the non-adsorbed part, and the non-adsorbed part is concentrated and dried at a pressure of 0.09MPa and a temperature of 65°C to obtain a crude pro...

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Abstract

The invention discloses a preparation method of high-purity 1-deoxynojirimycin. 1-deoxynojirimycin is enriched by using ammonium cation exchange resin, and the 1-deoxynojirimycin is pulped and purified by combining anion exchange resin and a hot solvent to prepare the high-purity 1-deoxynojirimycin. The use of a high-concentration acid liquor can be avoided, so that equipment in a production workshop is prevented from being corroded by acids, the production risk is reduced, the energy consumption can be reduced, the solvent loss can be reduced, the product yield can be increased, and finally,the product with the mass content of 1-deoxynojirimycin being greater than 98.0% can be prepared.

Description

technical field [0001] The invention relates to an alkaloid extraction and separation technology, in particular to a preparation method suitable for industrial production of high-purity 1-deoxynojirimycin. Background technique [0002] Existing mulberry leaf is the dry leaf of Morus alba L. of Moraceae plant, and mulberry is planted widely as a kind of economic plant, and its fruit, leaf, branch, root bark etc. are all used as medicine. "Compendium of Materia Medica" describes five different kinds of mulberry, that is, "there are several kinds of mulberry, including white mulberry, whose leaves are as big as a palm and thick; chicken mulberry, whose leaves are flowery and thin; son mulberry, which is mulberry first and then leaves; mountain mulberry, whose leaves are pointed and long. Those who are planted with seeds should not be divided as if they were divided by beading. The yellow clothes of the mulberry are called golden mulberry, and the wood will wither." "The Book of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/36
CPCC07D211/36Y02A50/30
Inventor 李名洁陈志元江丹王玉孙代华胡力飞王泽霞
Owner 劲牌持正堂药业有限公司
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