1-deoxynojirimycin preparing method suitable for industrial production

A deoxynojirimycin and drying technology, which is applied in the field of preparation of 1-deoxynojirimycin, can solve the problems of insufficient attention in the actual operation and cost control of production, large losses, and large investment in equipment, so as to improve the solvent dissolution efficiency , saving use and loss, and reducing production costs

Active Publication Date: 2014-08-06
HUNAN HUACHENG BIOTECH
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Problems solved by technology

[0003] At present, there are many methods for extracting 1-deoxynojirimycin (DNJ) from mulberry leaves. For example, Chinese patent application No. 200710067498.3 discloses a method for extracting 1-deoxynojirimycin from mulberry leaves. The method is to extract the mulberry leaves after crushing, acidify with inorganic acid, then pass through the cation exchange resin, elute with ammonia alcohol, and concentrate and dry to obtain a DNJ product with a content of more than 10%. Although the process is simple, the cation exchange resin , the loss is relatively large; the application number is 201210190238.6 Chinese patent application discloses a method for preparing mulberry leaf 1-deoxynojirimycin extract by using filter membrane and resin, the method is to extract mulberry leaf, concentrate, microporous filtration, After filtering through an organic ultrafiltration membrane, then passing through a macroporous adsorption resin and cation and anion exchange resins, and finally concentrating and drying the product, the product purity can reach more than 50%. , unfavorable for industrial production; the Chinese patent application with application number 201210411230.8 discloses a process for extracting and preparing 1-deoxynojirimycin from mulberry leaves. Macroporous resins and cation exchange resins can be concentrated, adsorbed on silica gel, desorbed and dried to obtain products with a purity of more than 70% of DNJ. This method has the disadvantages of complicated process, low yield and high cost.
[0004] As far as the above-mentioned methods are concerned, most of them are dedicated to improving the purity of 1-deoxynojirimycin, and have not paid enough attention to the actual operation and cost control of production. Therefore, there are few existing technologies that are really suitable for factory production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] This embodiment includes the following steps:

[0040] (1) Raw material pretreatment: crush 100kg of dry raw material mulberry leaves, and pass through a 24-mesh sieve to obtain 99.5kg of powder;

[0041] (2) Enzymolysis: Add 600kg of water to the powder obtained in step (1), raise the temperature to 50°C, then add 200g of combined enzyme (cellulose: pectinase = 4:1, w / w), keep the temperature Enzymolysis for 5 hours, filtering to obtain filter residue;

[0042] (3) Continuous combined extraction: Divide the filter residue obtained in step (2) into 4 parts and place them in 4 sets of extraction devices for continuous combined extraction. The filter residue in each extraction device is extracted 4 times, and the solvent for each extraction is 80% ethanol (containing 0.4% hydrochloric acid, 37.5% hydrochloric acid mass fraction) of 9 times the weight of dry raw materials, the extraction temperature is 85°C, and the extraction time is 2.2h. After extraction, combine the e...

Embodiment 2

[0048] This embodiment includes the following steps:

[0049] (1) Raw material pretreatment: crush 100kg of dry raw material mulberry leaves and pass through a 24-mesh sieve to obtain 99.5kg of powder;

[0050] (2) Enzymolysis: Add 800kg of water to the powder obtained in step (1), raise the temperature to 50°C, then add 50g of combined enzyme (cellulose: pectinase = 2:1, w / w), keep the temperature Enzymolysis for 3 hours, filtered to obtain filter residue;

[0051] (3) Continuous combined extraction: Divide the filter residue obtained in step (2) into 3 parts and place them in 3 sets of extraction devices for continuous combined extraction. The filter residue in each extraction device is extracted 3 times, and the solvent for each extraction is The volume fraction of 50% ethanol (including 0.2% hydrochloric acid by volume fraction and 37.5% hydrochloric acid by volume fraction) is 6 times the weight of dry raw materials, the extraction temperature is 70°C, and the extraction...

Embodiment 3

[0057] This embodiment includes the following steps:

[0058] (1) Raw material pretreatment: crush 100kg of dry raw material mulberry leaves, and pass through a 24-mesh sieve to obtain 99.6kg of powder;

[0059] (2) Enzymolysis: Add 600kg of water to the powder obtained in step (1), raise the temperature to 50°C, then add 100g of combined enzyme (cellulose: pectinase = 4:1, w / w), keep the temperature Enzymolysis for 5 hours, filtering to obtain filter residue;

[0060] (3) Continuous combined extraction: Divide the filter residue obtained in step (2) into 3 parts, and place them in 3 sets of extraction devices for continuous combined extraction, extract the filter residue in each extraction device 4 times, each extraction solvent is 80% ethanol with a volume fraction of 9 times the weight of dry raw materials (containing 0.4% hydrochloric acid by volume, 37.5% hydrochloric acid mass fraction), the extraction temperature is 85°C, and the extraction time is 2.2h. After extracti...

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Abstract

A 1-deoxynojirimycin preparing method suitable for industrial production comprises the following steps: (1) raw material pre-treatment: crushing the dry mulberry leaf raw material; (2) enzymelysis: adding water into powder, raising the temperature, adding a combined enzyme for enzymelysis, and filtering; (3) continuous combined extraction: performing continuous combined extraction on filter residues by using 3-4 extracting devices, mixing extracting solutions, and filtering; (4) alcohol precipitation and centrifugation: performing pressure-reduction concentration to 1/3-1/2 of the original volume, cooling, adjusting pH, adding an alcohol solution, stirring, performing still standing, and centrifuging by using a tube centrifuge; (5) membrane filtration: at 25-35 bar pressure at room temperature, ultrafiltering by using an organic ultrafiltration membrane, and then at 0.5-1.5 MPa pressure at room temperature, nano-filtering by using a nanofiltration membrane; (6) concentrating; (7) drying. By using the 1-deoxynojirimycin preparing method, the loss of a solvent can be reduced to a large extent, the energy consumption can be reduced and the product yield can be increased; therefore, the 1-deoxynojirimycin preparing method is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of 1-deoxynojirimycin, in particular to a preparation method of 1-deoxynojirimycin suitable for industrial production. Background technique [0002] Mulberry leaf, also known as iron fan, is the dry leaf of Moraceae mulberry (Morus alba L.), which is widely distributed and planted in large quantities in my country. For a long time, mulberry leaf is mainly used in two aspects, one is the breeding of silkworms, One is traditional Chinese medicine, which is believed to have the functions of dispelling wind-heat, clearing liver and improving eyesight, cooling blood to stop bleeding, clearing lung and moistening dryness, etc. As a medicinal and edible plant approved by the Ministry of Health, with the deepening of research, it has been shown that mulberry leaves contain active substances such as flavonoids, alkaloids, amino acids, vitamins and minerals, among which a piperidine alkaloid 1-Deoxynojirimycin (DNJ) ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D211/46
CPCC07D211/46
Inventor 唐方华黄华学刘永胜
Owner HUNAN HUACHENG BIOTECH
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