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Technological method for extracting 1-deoxynojirimycin from mulberry leaf

A technology of deoxynojirimycin and process method, which is applied in the field of extraction and preparation of 1-deoxynojirimycin, which can solve the problems of solvent residue and achieve the effect of reducing the amount of treatment

Inactive Publication Date: 2015-04-08
上海丝绸集团股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a process for extracting and preparing 1-deoxynojirimycin from mulberry leaves, to prepare 1-deoxynojirimycin products with a content of more than 70%, and to solve the problem of solvent residue in the final product

Method used

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  • Technological method for extracting 1-deoxynojirimycin from mulberry leaf
  • Technological method for extracting 1-deoxynojirimycin from mulberry leaf

Examples

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Embodiment 1

[0028]1 kg of mulberry leaves was crushed, passed through a 20-mesh sieve, extracted twice with 10 kg of deionized water, the temperature was controlled at about 95°C, and extracted twice, the first extraction was 2 hours, and the second extraction was 1 hour. Combine the extracts, filter, and concentrate to about 800ml to obtain liquid A; then add 3000ml of 95% ethanol to liquid A, let it stand for 18 hours, filter to remove the precipitate, put the mother liquor in a rotary evaporator to concentrate, adjust the temperature of the water bath to 60°C, When the vacuum degree is above 0.05MPa, ethanol is recovered and concentrated to 800ml to obtain liquid B.

[0029] Soak 1000g of macroporous resin in 4000ml of ethanol for 6 hours, then soak in 3000ml of ethanol for 3 hours, then soak in 2000ml of ethanol for 2 hours, wash with alcohol to remove impurities, then wash with water to remove the ethanol remaining in the macroporous resin until there is no alcohol smell , and finall...

Embodiment 2

[0035] 800g of mulberry leaves were crushed, passed through a 30-mesh sieve, and refluxed with 12kg of 20% ethanol for 3 times, the temperature was controlled at about 85°C, the first extraction was 2 hours, the second time was 1 hour, the third time was 1 hour, combined The extract was filtered and concentrated to about 1600ml to obtain liquid A; then, 1600ml of absolute ethanol was added to liquid A, left for 10 hours, and the precipitate was removed by centrifugation. When the concentration is above 0.05MPa, recover ethanol and concentrate to 1600ml to obtain liquid B.

[0036] 1600g macroporous adsorption resin is first soaked in 3000ml of ethanol for 5 hours, then soaked in 2000ml of ethanol for 3 hours, then soaked in 1600ml of ethanol for 1 hour. , and finally wet packed into the chromatography column (diameter x height, 60mm x 900mm). Add liquid B to the treated D101 macroporous adsorption resin chromatography column, let it stand for 4 hours, then elute with deionize...

Embodiment 3

[0042] Crush 400g of mulberry leaves, pass through a 20-mesh sieve, extract twice with 6kg of deionized water, control the temperature at about 90°C, extract for 2 hours for the first time, and 1 hour for the second time, combine the extracts, filter, and concentrate to 800ml , then add 3200ml of 95% ethanol to the concentrated solution, leave it for 12 hours, filter to remove the precipitate, put the mother liquor into a rotary evaporator to concentrate, adjust the temperature of the water bath to 75°C, and the vacuum degree to 0.07MPa, recover the ethanol, concentrate to 800ml, that is Get liquid B.

[0043] Soak 1200g macroporous resin in 4000ml of ethanol for 4 hours, then soak in 2000ml of ethanol for 2 hours, then soak in 1500ml of ethanol for 1 hour. , and finally wet packed into the chromatographic column (diameter x height, 80mm x 650mm). Add liquid A to the treated HPD-722 macroporous adsorption resin chromatography column, let it stand for adsorption for 3 hours, t...

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Abstract

The invention relates to a technological method for extracting 1-deoxynojirimycin from mulberry leaves, which is a technological method for extracting and separating 1-deoxynojirimycin with content being more than 70 percent from mulberry leaves. The technological method comprises the following steps of: conducting water extraction and alcohol precipitation on mulberry leaves, removing impurities by using macroporous resin, enabling mulberry leaf alkaloid to be enriched by cations, conducting gradient elution through silica gel column chromatography, and conducting vacuum drying to finally obtain the 1-deoxynojirimycin product. The technological method provided by the invention has the advantages that the technological process is simple, the obtained product does not contain residual organic solvent, the fillers for silica gel column chromatography are low in cost and can be repetitively used, the cost is reduced, special equipment is not needed in the entire technological process, the operation is simple and feasible to conduct and the technological method is very suitable for industrial production.

Description

technical field [0001] The invention relates to a process method for extracting and preparing 1-deoxynojirimycin from mulberry leaves; it belongs to the technology of extracting and separating pharmacological active ingredients from natural products. Background technique [0002] Mulberry leaf is the leaf of Morus alba L., a plant of Moraceae. It is one of the traditional Chinese medicinal materials in my country. The theory of traditional Chinese medicine believes that it has the functions of dispelling wind-heat, clearing lung and moistening dryness, calming liver yang, clearing liver and improving eyesight, and cooling blood. Hemostasis and other effects. Modern scientific research shows that mulberry leaves contain minerals, vitamins, amino acids, flavonoids, alkaloids, polysaccharides and other chemical components, which have physiological effects such as lowering blood sugar, lowering blood pressure, anti-aging, antibacterial, and antiviral; In particular, the polyhydr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/46
Inventor 王济强王小峰殷妮张菁赵嵩朱桂秀
Owner 上海丝绸集团股份有限公司
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