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Method for extracting and separating high-purity 1-Deoxynojirimycin from folium mori

A deoxynojirimycin, high-purity technology, applied in the field of extraction and separation of active components of traditional Chinese medicine, can solve the problems of low 1-deoxynojirimycin content, cost reduction, etc., and achieves the advantages of avoiding solvent residues, avoiding repeated operations, and operating safety. Effect

Inactive Publication Date: 2011-06-22
HANGZHOU HUIYUAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the inventive method does not need to add a flocculant, it can reduce the cost and increase the content while ensuring that no exogenous substances are brought in during the post-treatment process. After the acidification solution is concentrated, it is directly separated by domestic ion exchange column chromatography. The cost is greatly reduced; the biggest defect of this patent is that the content of the prepared 1-deoxynojirimycin is low, only about 10%
[0005] However, there is no report about the whole process of extracting and separating high-purity 1-DNJ from mulberry leaves

Method used

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  • Method for extracting and separating high-purity 1-Deoxynojirimycin from folium mori
  • Method for extracting and separating high-purity 1-Deoxynojirimycin from folium mori

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] refer to figure 1 , a method for extracting and separating high-purity 1-deoxynojirimycin from mulberry leaves, comprising the following sequential steps:

[0036] The mulberry leaf medicinal material is pulverized and passed through a 40-mesh sieve;

[0037] Take 10kg of raw material powder and use 75% ethanol to extract twice at 60°C (the solvent times are 10 times and 8 times respectively), 1 hour each time;

[0038] Combine the extracts, centrifuge, and concentrate under reduced pressure at 60°C to about 20L;

[0039] The concentrated solution is passed through an ultrafiltration membrane, the ultrafiltrate is added with hydrochloric acid to adjust the pH to 3.0, and centrifuged to obtain an acidified solution;

[0040] Take 2L of the acidification solution, put it on a 001×8 resin column with a column volume of 1L, wash it with water for 3 times the column volume, and then use 3 times the column volume concentration to elute with 1.0% ammonia water, the flow rate...

Embodiment 2

[0045] Get 3L of the ammonia eluent in Example 1, and adjust to neutrality with hydrochloric acid;

[0046] The HP20 macroporous resin column with a column volume of 1L was washed with water for 2 times the column volume, and then gradient eluted with an ethanol solution with a concentration of 2 times the column volume of 10-70%, and the flow rate was 1 times the column volume / h, and collected in steps eluent;

[0047] Combine eluents with an ethanol concentration of 20%-40%, concentrate under reduced pressure (55°C-60°C), and dry in vacuum to obtain a crude product with a content of 52.8%, with a total conversion rate of 84.2% and a yield of 0.43% ;

[0048] Take 8.0g of the obtained crude product, dissolve it in 200ml of absolute ethanol, pass it through a basic alumina adsorption column, collect the effluent, concentrate under reduced pressure under vacuum (55°C-60°C) to an appropriate volume, crystallize at room temperature, and recrystallize 1-2 times , the 1-DNJ refin...

Embodiment 3

[0050] Get 3L of the ammonia eluent in Example 1, and adjust to neutrality with hydrochloric acid;

[0051]The CAD-40 macroporous resin column with a column volume of 1L was washed with water for 2 times the column volume, and then gradient eluted with an ethanol solution with a concentration of 10-70% for 2 times the column volume, and the flow rate was 1 times the column volume / h. Step to collect the eluate;

[0052] Combine eluents with an ethanol concentration of 20%-40%, concentrate under reduced pressure (55°C-60°C), and dry in vacuum to obtain a crude product with a content of 54.1%, with a total conversion rate of 86.1% and a yield of 0.42% ;

[0053] Take 8.0g of the obtained crude product, dissolve it in 200ml of absolute ethanol, pass it through a basic alumina adsorption column, collect the effluent, concentrate under reduced pressure under vacuum (55°C-60°C) to an appropriate volume, crystallize at room temperature, and recrystallize 1-2 times , to obtain a refi...

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Abstract

The invention relates to a technology for extracting and separating active ingredients of traditional Chinese medicines, in particular to a method for extracting and separating high-purity 1-deoxynojirimycin from folium mori, which comprises the following steps of: extracting a powder material by using an aqueous solvent, filtering off dregs, and centrifuging the material to obtain extracting solution; concentrating the extracting solution until ethanol does not exist, and filtering by using an ultrafiltration membrane; regulating the pH to be 3.0-4.0 by using inorganic acid, precipitating, and centrifuging to removing impurities; applying acidified feed to a strong acid cation resin column, washing with water, and eluting by using ammonia water; applying feed liquid to a porous resin column, washing with water, performing gradient elution by using ethanol with different concentrations, and collecting target eluent; concentrating the target eluent under reduced pressure, and drying to obtain a crude product; dissolving the crude product by using absolute ethanol, making the solution pass through an alkaline adsorbing column to remove impurities, and collecting effluent liquid; and concentrating the effluent liquid under reduced pressure, and performing normal temperature crystallization and recrystallization to obtain the refined 1-DNJ product. In the whole technological process, except ethanol, other organic solvents are not used, the operation is safe, and the 1-DNJ content can reach 98.3 percent.

Description

technical field [0001] The invention relates to a technique for extracting and separating effective components of traditional Chinese medicine, in particular to a method for extracting and separating high-purity 1-deoxynojirimycin from mulberry leaves. Background technique [0002] Mulberry leaf is the leaf of the Moraceae (Moraceae) Morus plant (Morus L.). It is a medicinal and edible plant announced by the Ministry of Health. It is cultivated and produced in most parts of the country, with the largest output in the main sericulture production areas in the south, such as Jiangsu, Guangxi, Zhejiang, Anhui, Sichuan, etc. There are 15 species and 4 varieties of Morus in my country, among which white mulberry (Morus alba) is mostly used as medicine. Mulberry leaf is rich in resources in my country, and it is also a commonly used traditional Chinese medicine in ancient medical prescriptions. Mulberry has been recorded in "The Book of Songs", and the use of mulberry leaves as m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/46
Inventor 马全民聂复礼李雪斌杜大庆
Owner HANGZHOU HUIYUAN IND
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