Method for extracting shikimic acid and shikimic acid extract

Abstract

The invention provides a method for extracting shikimic acid and a shikimic acid extract. The method for extracting shikimic acid comprises the following steps: (1) carrying out membrane filtration, heating and alkali regulation treatment on fermentation liquor containing shikimic acid so as to obtain a first treated liquid; (2) carrying out acid regulation and concentration treatment on the firsttreated liquid to obtain a second treated substance; (3) carrying out desalination and decolorization treatment on the second treated substance to obtain a third treated liquid; (4) carrying out crystallization treatment on the third treated liquid, and collecting obtained crystals; and (5) washing and drying the crystals to obtain the shikimic acid extract. According to the method for extractingthe shikimic acid, the high-purity shikimic acid extract can be obtained without adopting a complex resin adsorption process, and the purity can reach up to 99%. Moreover, the method is simple and convenient to operate, low in production cost and capable of realizing large-scale production and application.

Description

technical field [0001] The invention relates to the field of biomedicine. Specifically, the present invention relates to a method for extracting shikimic acid and a shikimic acid extract. Background technique [0002] Shikimic acid (3,4,5-3 hydroxy-1-cyclohexene-1-carboxylic acid), English name: shikimic acid (SA), is the key intermediate in the synthesis of antiviral drug oseltamivir phosphate (Kewei) body. Shikimic acid is white needle-like crystal, easily soluble in water, insoluble in organic solvents such as petroleum ether, with a bitter smell and a melting point of 185-187°C. Shikimic acid is a key intermediate in the biosynthetic pathway of aromatic amino acids in organisms, and it is also an important precursor for the synthesis of indole derivatives, alkaloids, and chiral drugs (such as antiviral drugs), and has a wide range of medicinal value. [0003] Shikimic acid widely exists in a variety of plants, and its content is relatively high in the Magnoliaceae sta...

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Problems solved by technology

But in general, the steps of extracting shikimic acid from plants are cumbersome, the source of raw materials is unstable, and is often affected by conditions such as the climate of the place of production, which is not conducive to increasing the production of shikimic acid in industry

[0004] In recent years, the technology of shikimic acid synthesis by microbial fermentation has become more and more mature, but there are many impurities in the fermentation broth, which limit the purification and separation of shikimic acid (such as: proteins, pigments, inorganic salts and shikimic acid structural analogues ), especially 3-dehydroshikimic acid (DHSA), which is unavoidably produced in biosynthesis, is very difficult to separate due to its similar properties to shikimic acid

[0005] Commonly used methods for extracting shikimic acid in fermented liquid mainly include resin separation and organic solvent extraction. For example, patent CN102584571 discloses a method for preparing shikimic acid with anion resin, but there is no other pretreatment after ceramic membrane and ultrafiltration membrane treatment. In the purification step, the anion exchange resin is directly used for adsorption and elution purification. There are problems such as low processing capacity of the anion exchange resin, low chromatographic purity of the obtained eluent, and inability to separate impurities with similar structures, and mixed solvents are used for crystal washing. Recycling is difficult, which increases the pressure on environmental protection, solvent recovery is difficult, and is not suitable for industrial production

CN109721487 has announced the method for separating shikimic acid in fermented liquid with anion-cation exchange resin, can obtain shikimic acid with higher purity, but this technique is still limited by the loading capacity of resin, and the equipment investment of column chromatography is large, resin pretreatment And regeneration produces a large amount of waste water, it is difficult to reduce production costs, and the environment is under great pressure

Wang Hui and others reported the method of using anion and cation exchange resins to jointly prepare shikimic acid crystals. The crystal purity can reach 98%, but there are also problems such as low resin treatment capacity and low total yield, and it is not feasible for industrialization.

[0006] In addition to resin separation, foreign patents also report the method of organic solvent extraction. As described in the patent US20160176799, n-butanol is used to extract shikimic acid in the fermentation broth. Although shikimic acid with high purity can be prepared, because shikimic acid is in The solubility in n-butanol is much lower than that in water, resulting in low extraction efficiency and difficult to realize industrial production

Patent WO0206203 also uses organic solvents to extract and prepare shikimic acid. This method requires freeze-drying, and the solvent used is acetone. Its solubility for shikimic acid is low, and the overall energy consumption is large, making it difficult to achieve large-scale industrial applications.

[0007] Therefore, the current method of extracting shikimic acid remains to be studied

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