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Method for extracting and separating 1-deoxynojirimycin with high purity from natural products

A technology for deoxynojirimycin and natural products, which is applied in the field of traditional Chinese medicine and achieves the effects of obvious economic benefit, low equipment cost and mature technology

Inactive Publication Date: 2012-05-23
CHENGDU GOLD DOCTOR TECH HEALTH IND +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For extracting and separating high-purity (over 98%) 1-deoxynojirimycin from natural products and simultaneously preparing crude 1-deoxynojirimycin (purity over 35%), protein feed, crude flavonoids and refined polysaccharides (over 90%) method, which has not been reported in existing patents
In addition, the present invention has been carried out in a pilot test (feeding 500kg), and in the existing patents for the preparation of 1-deoxynojirimycin and related by-products, there is no report that has entered the pilot test

Method used

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  • Method for extracting and separating 1-deoxynojirimycin with high purity from natural products
  • Method for extracting and separating 1-deoxynojirimycin with high purity from natural products
  • Method for extracting and separating 1-deoxynojirimycin with high purity from natural products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1 Extraction of high-purity 1-deoxynojirimycin and preparation of by-products from mulberry leaves

[0046] A. Extraction and separation of high-purity 1-deoxynojirimycin:

[0047]The mulberry leaves are washed and dried, crushed, and passed through a 40-mesh sieve. Weigh 50kg of mulberry leaf powder, add 400L 65% ethanol, ultrasonically extract at 60°C 800HZ for 30min, filter, add 200L 65% ethanol to the filter residue, extract ultrasonically at 60°C 800HZ for 30min, filter, combine the filtrates, and filter the residue for use.

[0048] Add 2 mol / L hydrochloric acid to the filtrate in 1), adjust pH=2, concentrate under reduced pressure to 20 L, filter with suction, and filter residue for use. Add the filtrate to 100kg717 anion exchange resin, stir for 15min, let it sit for 6h, then release the liquid, add the effluent to the original anion resin, repeat 3 times, add 300L water to elute, collect the effluent and washing water, and concentrate to 20L.

[0049]...

Embodiment 2

[0058] Example 2 Extraction of high-purity 1-deoxynojirimycin and preparation of by-products from silkworm excrement

[0059] A. Extraction and separation of high-purity 1-deoxynojirimycin:

[0060] 1) Take the 5th instar silkworm excrement, dry it, crush it, and pass it through a 40-mesh sieve. Weigh 400g of silkworm excrement powder, add 4000mL 65% ethanol, ultrasonically extract at 60°C 1500HZ for 25min, filter, add 2400mL 65% ethanol to the filter residue, extract ultrasonically at 60°C 1500HZ for 25min, filter, combine the filtrates, and filter the residue for use.

[0061] Add 2 mol / L hydrochloric acid to the filtrate in 1), adjust pH=3, concentrate under reduced pressure to 200 mL, filter with suction, and filter the residue for use. Add the filtrate to 1kg717 anion exchange resin, stir for 15min, let it sit for 6h, then release the liquid, add the effluent to the original anion resin, repeat 3 times, slowly add 3L water to elute, collect the third effluent and washing...

Embodiment 3

[0071] Embodiment 3 extracts high-purity 1-deoxynojirimycin from mulberry fruit:

[0072] 1) The mulberries are dried and pulverized, and passed through a 40-mesh sieve. Weigh 2kg of mulberry powder, add 15L 80% methanol, 70°C 1200HZ ultrasonic extraction for 20min, filter, add 10L 80% methanol to the filter residue, 70°C 1200HZ ultrasonic extraction for 20min, filter, combine the filtrates, and filter residue for use.

[0073] 2) Add 2 mol / L sulfuric acid to the filtrate in 1), adjust pH=3, concentrate under reduced pressure to 1 L, filter with suction, and filter the residue for use. Add the filtrate to 5kg701 anion exchange resin, stir evenly, let the liquid release after 10 hours of stuffing, add the effluent to the original anion resin, repeat 3 times, add 20L water to elute, collect the third effluent and washing water, and concentrate to 1L.

[0074] Purify the concentrated solution in 2) by 5kg732 cation exchange resin column chromatography: after loading the sample, ...

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Abstract

The invention relates to the field of the traditional Chinese medicine, in particular to a method for extracting and separating 1-deoxynojirimycin (DNJ) with the purity higher than 98% from natural products comprising mulberry leaves, mulberry twigs, white mulberry root-bark, mulberry fruit and silkworm litter and also preparing a 1-deoxynojirimycin crude product (with the purity more than 35%), protein feeds, crude flavone and refined polysaccharide (with the purity more than 90%). The method mainly comprises the following steps: extracting a raw material of dry powder by a hydrophilic solvent, soaking by anion exchange resin after acidizing and concentrating extracting liquid, carrying out chromatography by a cation exchange column after concentrating effluent liquid and water washing liquid, extracting by an organic solvent, recrystallizing, carrying out chromatography by a gel column and purifying. The content of the 1-deoxynojirimycin in the obtained product is not less than 98%,and the concrete execution already enters intermediate test.

Description

technical field [0001] The invention relates to the field of traditional Chinese medicine, namely a method for extracting and separating high-purity 1-deoxynojirimycin (1-Deoxynojirimycin, DNJ) from natural products and preparing high value-added by-products. Background technique [0002] 1-Deoxynojirimycin (1-Deoxynojirimycin, DNJ) is a piperidine alkaloid, the chemical name is 3,4,5-trihydroxy-2-hydroxymethyltetrahydropyridine (structural formula 1), CAS number 19130- 96-2, the molecular formula is C 6 h 13 NO 4 , with a molecular weight of 163. DNJ has high-efficiency physiological activity, can be used to treat diseases such as diabetes, obesity, and viral infection, can inhibit tumors, has inhibitory effect on a-glucoamylase, and can be used as a carrier for the enzyme synthesis of high-purity maltose. [0003] [0004] Structural formula 1 Chemical structure of 1-deoxynojirimycin [0005] Figure 1The chemical constitution of 1-DNJ [0006] Among the existing p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/46C07D311/30C08B37/00A23K1/14A23K10/30A23K20/10
Inventor 杨茹卢朝华
Owner CHENGDU GOLD DOCTOR TECH HEALTH IND
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