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Method for continuously extracting and separating 1-deoxynojirimycin (DNJ) and flavone from folium mori

A technology of deoxynojirimycin and mulberry leaves, applied to medical preparations containing active ingredients, pharmaceutical formulas, plant/algae/fungus/moss ingredients, etc., can solve problems such as difficult to remove, low active ingredients, easy to lose, etc. Achieve the effects of reducing viscosity and hygroscopicity, maintaining biological activity, and improving product quality

Active Publication Date: 2010-03-17
GUANGDONG APOLLO GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that a high-speed centrifuge is used for material-liquid separation, which is expensive in industry; in addition, the material liquid is separated from flavonoids through a macroporous resin, and then the alkaloids are extracted through a cationic resin, which is easy to lose precious and relatively low content. Low active ingredient 1-deoxynonomycin (DNJ) (0.2%-0.4% in mulberry leaves)
But its disadvantage is that this process uses organic solvents such as chloroform and n-hexane when preparing alkaloids, which are toxic and difficult to remove from the product, and are not suitable for large-scale industrial production
The advantage is that the separated product can be easily obtained, but the disadvantage is that the production step needs to cool the extract to 10°C to 30°C, the conditions are relatively harsh, and methanol, diethylamine, triethylamine, etc. are used in the process Toxic and flammable organic solvents are not conducive to clean production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The method for producing the mulberry leaf extract of the present invention has the following steps:

[0028] (a) Weigh 20Kg of mulberry leaf powder and place it in an extraction tank, add 160L of 60% ethanol, stir for 2h at 60°C, and filter with a centrifuge to obtain the filtrate;

[0029] (b) Add 160L of 60% ethanol to the filter residue, repeat the extraction once and filter according to the above conditions, combine the filtrates obtained twice, concentrate under reduced pressure at 70°C with a vacuum concentration tank, and recover ethanol;

[0030] (c) Dilute the concentrated solution to 100L with water, adjust the pH to 3 with hydrochloric acid, heat it to 55°C and keep it warm, add 4L of ZTC1+1 flocculant A component (1%) while stirring, and stir once every half hour; 2 hours Finally, add 2L of ZTC1+1 flocculant B component (1% viscose, prepared with 1% acetic acid), stir evenly, and stir again after half an hour, stop the heat preservation, and let stand overn...

Embodiment 2

[0036] The method for producing the mulberry leaf extract of the present invention has the following steps:

[0037] (a) Weigh 10Kg of mulberry leaf powder and place it in an extraction tank, add 400L of 40% ethanol, stir for 1h at 70°C, and filter with a centrifuge to obtain the filtrate;

[0038] (b) Add 40% ethanol to the filter residue, repeat the extraction once and filter according to the above conditions, combine the filtrate obtained twice, concentrate in a vacuum at 70° C. in a vacuum concentration tank, and recover ethanol;

[0039] (c) Dilute the concentrated solution to 60L with water, adjust the pH to 5 with hydrochloric acid, add 5L of 1% chitin solution, stir evenly, and let stand overnight;

[0040] (d) Press filtration to remove the precipitate, and the filtrate is pumped into 2 Dowex-50 cationic resin columns (D×H=10cm×100cm) connected in series, and then flows through 1 HPD-400 macroporous resin column (D ×H=10cm×60cm);

[0041] (e) After the filtrate is a...

Embodiment 3

[0045] The method for producing the mulberry leaf extract of the present invention has the following steps:

[0046] (a) Weigh 20Kg of mulberry leaf powder, place it in an extraction tank, add 400L of 80% ethanol, stir for 2h at 50°C, and filter with a centrifuge to obtain the filtrate;

[0047] (b) Add 200L of 80% ethanol to the filter residue, repeat the extraction once and filter according to the above conditions, combine the filtrates obtained twice, concentrate in a vacuum at 50° C. in a vacuum concentration tank, and recover ethanol;

[0048] (c) Dilute the concentrated solution with water to 100L, adjust the pH to 5 with acetic acid, heat it to 55°C and keep it warm, add 4L of ZTC1+1 flocculant A component (1%) while stirring, and stir once every half hour; 2 hours Finally, add 2L of ZTC1+1 flocculant B component (1% viscose, prepared with 1% acetic acid), stir evenly, and stir again after half an hour, stop the heat preservation, and let stand overnight;

[0049] (d) ...

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PUM

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Abstract

The invention relates to a method for continuously extracting and separating 1-deoxynojirimycin (DNJ) and flavone from folium mori; the key points are that: folium mori and ethanol are mixed, and extracted and filtered centrifugally, and then flocculating agents are added for flocculation and precipitation after being concentrated; the precipitation is removed, and the filterate is added in a plurality of cation exchange resin columns which are communicated, and flows through a macroporous absorption resin column connected with the resin columns in series; after the filtrate adding is finished, the filtrate is washed until outflow liquid from the macroporous absorption resin column is colourless, and then the macroporous absorption resin column is disconnected, and then the 1-deoxynojirimycin (DNJ) is eluated with ammonia water or ammoniac ethanol solution from the cation exchange resin columns; the eluate is eluated by the cation exchange resin columns again, the operation is repeated, and then the eluate is collected, is concentrated and filtered with a 80D nanofiltration membrane and then is spray-dried, so as to obtain claybank powdery 1-deoxynojirimycin (DNJ). 3-10 percent ofalcohol is used for washing the macroporous absorption resin column to remove colloidal impurities, and then 50-70 percent of alcohol is used for washing flavone, the claybank eluate is collected, decompression and concentration are carried out to recover alcohol, and then spray-drying is carried out to obtain the claybank powdery folium mori general flavone.

Description

technical field [0001] The invention relates to a method for continuously extracting and separating 1-deoxynojirimycin (DNJ) and flavonoids from mulberry leaves. Background technique [0002] Mulberry leaf is the dry leaf of Moraceae plant mulberry, which is cultivated or wild, and has strong adaptability to soil, and it is mostly produced in most parts of the country. Bitter in the mouth, sweet, cold in nature. Studies have found that mulberry leaves have anti-inflammatory and hypoglycemic effects pharmacologically, and can lower blood fat and diuresis. Mulberry leaves have the above activities and pharmacological effects, mainly because their components contain 1-deoxynojirimycin (DNJ), flavonoids and other components, so it is very necessary to extract them from mulberry leaves for concentrated use . [0003] 1-Deoxynojirimycin (DNJ) is a strong α-glucosidase inhibitor, which inhibits α-glucosidase in the small intestine to decompose disaccharides such as sucrose and m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/46A61K36/605A61P3/10A61P9/00A61K127/00
Inventor 杭伟锋鲍玲刘钢邓国江张全才
Owner GUANGDONG APOLLO GRP
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