1-deoxynojirimycin preparing method suitable for industrial production

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) ...

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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.