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Purification method of deoxynojirimycin

A technology of deoxynojirimycin and purification method, which is applied in the field of biology and new medicine, can solve problems such as difficulty in meeting medical application standards, difficulty in realizing industrialization promotion, and destruction of target product structure, so as to reduce extraction cost, low cost, and equipment typical effect

Active Publication Date: 2012-06-13
中科医药行业生产力促进中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are few patents related to 1-DNJ extraction and purification in China. Among them, the patent application number 200410048393.X provides a 1-DNJ decoction extraction method. The method is simple in process and high in yield. It is easy to cause damage to the structure of the target product and affect the activity of the product; the patent application number 200710067498.3 provides a 1-DNJ dilute acid leaching extraction method, which is easy to operate and suitable for industrial production, but the 1-DNJ in the final product The content can only reach 10%, which is difficult to meet the application standards of the pharmaceutical industry; application number 20110038204.0 provides a 1-DNJ alcohol extraction method, which only uses ethanol as an organic solvent in the entire process, and is safe to operate , while the purity of 1-DNJ is high, but because the content of 1-DNJ in mulberry leaves is only about 0.2%, this invention does not provide a method for utilizing the waste extraction, and it is difficult to realize industrialization and popularization only by preparing a product of 1-DNJ

Method used

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  • Purification method of deoxynojirimycin
  • Purification method of deoxynojirimycin

Examples

Experimental program
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Effect test

Embodiment 1

[0029] After removing impurities and drying the mulberry leaves, crush them through a 40-mesh sieve, take 1kg of mulberry leaf powder, add 40L of 65% ethanol to soak for 30 minutes, and then ultrasonically extract 3 times, each ultrasonic power 125W, temperature 70°C, time 30min, suction filtration to obtain corresponding solid and liquid phases.

[0030] (1) Preparation of 1-deoxynojirimycin

[0031] The liquid phase obtained by ultrasonic crushing and centrifugation of mulberry leaves is recovered with a rotary evaporator and concentrated to a small volume, and the precipitate is removed by centrifugation. The supernatant is passed through a chromatographic column equipped with 732H cationic resin, and washed with distilled water until the effluent is colorless. , eluted with 0.25mol / L ammonia water, the elution rate was 1 times the column volume / h, the elution rate was 1-2mL / min, and the eluate was collected.

[0032] Concentrate the ammonia water eluate to about 1L, adjus...

Embodiment 2

[0039] After removing impurities and drying the mulberry leaves, crush them through a 40-mesh sieve, take 1kg of mulberry leaf powder, add 40L of 60% ethanol to soak for 40min, and extract by ultrasonic wave for 3 times, each time with ultrasonic power of 125W, temperature 70°C, time 30min, and suction filtration to obtain the corresponding solid and liquid phases.

[0040] (1) Preparation of 1-deoxynojirimycin

[0041] The liquid phase part obtained by ultrasonic crushing and centrifugation of mulberry leaves is recovered with a rotary evaporator and concentrated to a small volume, and the precipitate is removed by centrifugation. Until the color is gone, elute with 0.25mol / L ammonia water, the elution rate is 1 times the column volume / h, the elution rate is 1-2mL / min, and the eluate is collected.

[0042]Concentrate the ammonia water eluate to about 1L, adjust the pH value to 7.0 with 2mol / L acetic acid, add 0.25L chloroform extract in two times, stir evenly, let stand for ...

Embodiment 3

[0049] After removing impurities and drying the mulberry leaves, crush them through a 40-mesh sieve, take 1kg of mulberry leaf powder, add 40L of 65% ethanol to soak for 30min, and extract by ultrasonic wave 3 times, each time with ultrasonic power of 125W, temperature 70°C, time 30min, and suction filtration to obtain the corresponding solid and liquid phases.

[0050] (1) Preparation of 1-deoxynojirimycin

[0051] The liquid phase obtained by ultrasonic crushing and centrifugation of mulberry leaves is recovered with a rotary evaporator and concentrated to a small volume, and the precipitate is removed by centrifugation. The supernatant is passed through a chromatographic column equipped with 732H cationic resin, and washed with distilled water until the effluent is colorless. , eluted with 0.25mol / L ammonia water, the elution rate was 1 times the column volume / h, the elution rate was 1-2mL / min, and the eluate was collected.

[0052] Concentrate the ammonia water eluate to ...

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Abstract

The invention relates to a purification technology for extracting a compound from plants, particularly for extracting and separating high-purity 1-deoxynojirimycin from natural products, namely mulberry leaves, and simultaneously refining mulberry leaf polysaccharide. The method mainly comprises the following steps: pretreating raw materials, then dissolving the raw materials in an ethanol solution, performing ultrasonic extraction, concentrating extract liquid, then enabling the extract liquid to pass through cationic resin, concentrating eluate, and then extracting with an organic solvent, recrystallizing and carrying out gel filtration chromatography to prepare a refined product of the 1-deoxynojirimycin with the purity not lower than 98.5%. The process is simple to operate, low in cost, low in environmental pollution and typical in equipment and the materials are easy to obtain; therefore the process is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of biology and new medicine, and relates to extracting active compounds from plants, that is, extracting and separating high-purity 1-deoxynojirimycin and high value-added by-product mulberry leaf polysaccharide from mulberry leaves. Background technique [0002] 1-deoxynojirimycin (1-DNJ, hereinafter referred to as "1-DNJ") is a polyhydroxypiperidine alkaloid, also known as imino sugar because of its structure similar to monosaccharide, and its chemical name is 3,4 , 5-trihydroxy-2-hydroxymethyltetrahydropyridine, the chemical structure is as figure 1 As shown, the molecular formula is C 6 h 13 NO 4 , with a molecular weight of 163. 1-DNJ has a variety of biological activities and can be used to treat diseases such as diabetes, obesity, and viral infections. It can also inhibit tumors, inhibit α-glucoamylase, and can be used as a carrier for high Enzymatic synthesis of pure maltose. [0003] [0004...

Claims

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Application Information

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IPC IPC(8): C07D211/46C08B37/00
Inventor 殷红
Owner 中科医药行业生产力促进中心有限公司
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