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Method for continuously extracting and separating polysaccharides and 1-deoxynojirimycin from mulberry leaves

A technology of deoxynojirimycin and mulberry leaves, applied in the production of bulk chemicals, organic chemistry, etc., to achieve the effects of improving extraction rate, enhancing dissolution, and leaving no extractant residue

Inactive Publication Date: 2013-03-13
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, before extracting the hypoglycemic active components of mulberry leaves, the research on pretreatment of mulberry leaves to remove fat-soluble impurities and improve the extraction rate of polysaccharides and 1-deoxynojirimycin has not been reported.

Method used

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  • Method for continuously extracting and separating polysaccharides and 1-deoxynojirimycin from mulberry leaves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 400g of crushed mulberry leaf raw materials into the barrel and place the extraction cylinder, turn on the supercritical CO 2 Extraction device, extraction temperature 40°C, extraction pressure 30Mpa extraction for 80 minutes, CO 2 The flow rate is 30L / h. After the extraction, take out the barrel to obtain mulberry leaf residue, add 4L of 65% ethanol after drying, the ratio of solid to liquid is 1:10, stir at 80°C for 2h, and filter to obtain the filtrate. Add 4L of 65% ethanol to the filter residue to repeat extraction once and filter, combine the filtrate obtained twice, and concentrate to 200mL. Add 1.8L of 95% ethanol to the concentrated solution, let it stand for 4 hours, centrifuge, collect the precipitate, and dry at low temperature to obtain a light yellow powder, which is mulberry leaf polysaccharide. The content of mulberry leaf polysaccharide was determined by the phenol-sulfuric acid method to be 71%. The supernatant was concentrated to about 100 mL, a...

Embodiment 2

[0025] Add 400g of crushed mulberry leaf raw materials into the barrel and place the extraction cylinder, turn on the supercritical CO 2 Extraction device, extraction temperature 50°C, extraction pressure 40Mpa for 100 minutes, CO 2 The flow rate is 50L / h. After the extraction, the barrel was taken out to obtain mulberry leaf residue, after drying, 6 L of 60% ethanol was added, stirred at 80° C. for 2 h, and filtered to obtain the filtrate. Add 6L of 60% ethanol to the filter residue to repeat extraction once and filter, combine the filtrate obtained twice, and concentrate to 200mL. Add 1.5L of 95% ethanol to the concentrated solution, let it stand for 4 hours, centrifuge, collect the precipitate, and dry at low temperature to obtain a light yellow powder, which is mulberry leaf polysaccharide. The content of mulberry leaf polysaccharide was determined by the phenol-sulfuric acid method to be 69%. The supernatant was concentrated to about 100 mL, and passed through a pretrea...

Embodiment 3

[0027] Add 400g of crushed mulberry leaf raw materials into the barrel and place the extraction cylinder, turn on the supercritical CO 2 Extraction device, extraction temperature 35°C, extraction pressure 40Mpa extraction 120 minutes, CO 2The flow rate is 40L / h. After the extraction, the barrel was taken out to obtain mulberry leaf residue, after drying, 5 L of 75% ethanol was added, stirred at 80° C. for 2 h, and filtered to obtain the filtrate. Add 5 L of 75% ethanol to the filter residue to repeat extraction once and filter, combine the filtrate obtained twice, and concentrate to 200 mL. Add 1.6L of 95% ethanol to the concentrated solution, let it stand for 4 hours, centrifuge, collect the precipitate, and dry at low temperature to obtain a light yellow powder, which is mulberry leaf polysaccharide. The content of mulberry leaf polysaccharide was determined by the phenol-sulfuric acid method to be 74%. The supernatant was concentrated to about 100 mL, and passed through a...

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Abstract

The invention relates to a method for continuously extracting and separating polysaccharides and 1-deoxynojirimycin from mulberry leaves. The method comprises the following steps: grinding the mulberry leaves, carrying out supercritical CO2 extraction under certain conditions and collecting mulberry leaf dregs; after drying the mulberry leaf dregs, carrying out extraction through ethanol refluxing; concentrating the extracting solution, standing and drying the precipitate, thus obtaining a polysaccharide compound with the content being 60-80%; concentrating the supernatant and adsorbing active ingredients on resins via cation exchange resins; eluting the resins with water-containing ethanol and ammonia water; and concentrating the ammonia water eluent with a reversed-phase C18 silica gel based chromatographic column and drying the concentrated products, thus obtaining alkaloids in the mulberry leaves, wherein the content of 1-deoxynojirimycin in the alkaloids in the mulberry leaves is 80-86%. The detailed method refers to the specification. The method has the advantages that the process is simple, the extraction rate is high, the obtained products have higher purity, and the resins and silica gel used for purification are renewable, low in costs and beneficial to industrial popularization and application.

Description

technical field [0001] The invention relates to the field of extracting effective active ingredients from natural products and the modernization of traditional Chinese medicine, specifically a continuous extraction and separation of polysaccharides and 1-deoxynojirimycin (chemical name: (2R, 3R, 4R, 5S) from mulberry leaves. - 3,4,5-trihydroxy-2-hydroxymethyltetrahydropiperidine) method. Background technique [0002] Mulberry leaf is the leaf of Moraceae (Moraceae) plant mulberry (Morus alba L.). Since ancient times, it has been a commonly used Chinese herbal medicine in clinical medicine. Shu, "Compendium of Materia Medica", "Handbook of Chinese Herbal Medicine" and "Dictionary of Chinese Medicine". In recent years, modern pharmacological research has also fully proved that mulberry leaves have the functions of lowering blood sugar, lowering blood pressure, anti-aging and inhibiting cancer cells. In 1993, the Ministry of Health of my country announced that mulberry leaves...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/00C07D211/46
CPCY02P20/54
Inventor 李翠清王腾李继文张红
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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