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CN-121974785-A - Separation method of resveratrol fermentation liquor

CN121974785ACN 121974785 ACN121974785 ACN 121974785ACN-121974785-A

Abstract

The application provides a separation method of resveratrol fermentation liquor, which comprises the steps of (1) carrying out filter pressing treatment on resveratrol fermentation liquor to obtain second filter residues, wherein the filter pressing treatment comprises acid pressing on the fermentation liquor and then alkali pressing or alkali pressing on the fermentation liquor and then acid pressing, 2) carrying out extraction treatment on the second filter residues by adopting an organic solvent to obtain extract liquor, (3) carrying out washing treatment on the extract liquor to obtain washing liquor, wherein the washing treatment comprises the steps of sequentially carrying out alkali washing treatment and acid washing treatment on the extract liquor or sequentially carrying out acid washing treatment and alkali washing treatment on the extract liquor to obtain washing liquor, (4) carrying out decoloration and dehydration on the washing liquor and then concentrating to obtain concentrated liquor, and 5) carrying out crystallization treatment on the concentrated liquor to obtain resveratrol. The application can shorten the extraction period of the resveratrol without using a chromatographic method, reduce the cost and improve the purity and the yield of the resveratrol.

Inventors

  • FENG WEI
  • ZHAO YAN
  • GAO YUNXIA
  • Wang Menyue

Assignees

  • 北大医药重庆大新药业股份有限公司

Dates

Publication Date
20260505
Application Date
20251226

Claims (10)

  1. 1. The method for separating resveratrol fermentation liquor is characterized by comprising the following steps of: (1) Carrying out filter pressing treatment on resveratrol fermentation liquor to obtain second filter residues; wherein, the filter pressing treatment of resveratrol fermentation liquor comprises a first treatment or a second treatment: the first treatment process comprises the steps of adjusting the pH value of resveratrol fermentation liquor to be acidic, and then carrying out first filter pressing to obtain first filter residues; the second treatment process comprises the steps of adjusting the pH value of resveratrol fermentation liquor to be alkaline, and then carrying out third filter pressing to obtain first filter residues; (2) Extracting the second filter residue by adopting an organic solvent to obtain an extract containing resveratrol; (3) Washing the extract liquid to obtain a washing liquid containing resveratrol, wherein the washing treatment comprises sequentially performing alkali washing treatment and acid washing treatment on the extract liquid to obtain a washing liquid containing resveratrol, or sequentially performing acid washing treatment and alkali washing treatment on the extract liquid to obtain a washing liquid containing resveratrol; (4) Carrying out dehydration and decoloration treatment on the washing liquid containing resveratrol, and then concentrating to obtain concentrated liquid; (5) And (3) crystallizing the concentrated solution to obtain resveratrol.
  2. 2. The method for separating resveratrol fermentation broth according to claim 1, In the first treatment process, the pH value of the resveratrol fermentation liquor is regulated to be acidic, specifically, the pH value of the resveratrol fermentation liquor is regulated to be 2-4; and/or, in the first treatment process, adjusting the pH value of the resveratrol fermentation liquor to be acidic by adopting inorganic acid, wherein the inorganic acid comprises one or more of hydrochloric acid, oxalic acid, acetic acid, sulfuric acid and phosphoric acid; And/or, the first press filtration is plate-frame press filtration.
  3. 3. The method for separating resveratrol fermentation broth according to claim 1 or 2, wherein the first alkali liquor comprises an ammonium bicarbonate aqueous solution, wherein the mass concentration of ammonium bicarbonate in the ammonium bicarbonate aqueous solution is 5% -6%, and the ratio of the volume of the ammonium bicarbonate aqueous solution to the mass of the first filter residue is (1-2) L/1 Kg; And/or the first mixing treatment is carried out in a stirring state, and the time of the first mixing treatment is 2-3 hours; And/or, the second press filtration is plate-frame press filtration.
  4. 4. The method for separating resveratrol fermentation broth according to claim 1, In the second treatment process, the pH value of the resveratrol fermentation liquor is regulated to be alkaline, specifically, the pH value of the resveratrol fermentation liquor is regulated to be 8-9; and/or, in the second treatment process, adjusting the pH value of the resveratrol fermentation liquor to be alkaline by adopting a third alkaline substance, wherein the third alkaline substance comprises ammonium bicarbonate; And/or, the third filter pressing is plate-frame filter pressing.
  5. 5. The method for separating resveratrol fermentation broth according to claim 1 or 4, In the second treatment process, the first acid liquid comprises inorganic acid, and the inorganic acid comprises one or more of hydrochloric acid, oxalic acid, acetic acid, sulfuric acid and phosphoric acid; And/or the pH value of the first acid solution is 2-2.5, and the ratio of the volume of the first acid solution to the mass of the first filter residue is (1-2) L/1 Kg; And/or the second mixing treatment is carried out in a stirring state, and the time of the second mixing treatment is 2-3 hours; and/or, the fourth press filtration is plate-frame press filtration.
  6. 6. The method for separating resveratrol fermentation broth according to claim 1, The organic solvent comprises one or more of ethyl acetate, butyl acetate and n-butyl alcohol; And/or the extraction treatment process comprises the steps of adopting the organic solvent to extract the second filter residue twice, wherein the mass ratio of the volume of the organic solvent to the second filter residue is (3-5) L to 1Kg in each extraction process.
  7. 7. The method for separating resveratrol fermentation broth according to claim 1, Performing alkaline washing treatment on the extract by adopting a second alkali liquor, wherein the pH value of the second alkali liquor is 7-9; And/or, in the alkaline washing treatment process, the extraction liquid is washed for 2-3 times by adopting a second alkali liquid, and in each washing process, the volume ratio of the second alkali liquid to the extraction liquid is (0.8-1.2): 1; and/or carrying out alkaline washing treatment on the extract liquid by adopting a second alkaline liquid, wherein the second alkaline liquid comprises one or more of carbonate, bicarbonate, phosphate, acetate, metal hydroxide and ammonia water.
  8. 8. The method for separating resveratrol fermentation broth according to claim 1 or 7, Carrying out acid washing treatment on the extract liquid by adopting second acid liquid, wherein the pH value of the second acid liquid is 2-5; And/or, in the pickling treatment process, the extraction liquid is washed for 2-3 times by adopting a second acid liquid, and in each washing process, the volume ratio of the second acid liquid to the extraction liquid is (0.8-1.2): 1; And/or carrying out acid washing treatment on the extract liquid subjected to the alkali washing treatment by adopting a second acid liquid, wherein the second acid liquid comprises one or more of acetic acid, hydrochloric acid, phosphoric acid, sulfuric acid and oxalic acid.
  9. 9. The method for separating resveratrol fermentation broth according to claim 1, wherein a decolorizing agent and a drying agent are added to the washing liquid containing resveratrol to perform the decolorizing and dehydrating treatment, wherein the decolorizing agent comprises activated carbon, and the drying agent comprises anhydrous sodium sulfate and/or anhydrous magnesium sulfate; And/or, carrying out the concentration treatment by adopting a rotary steaming mode.
  10. 10. The method for separating resveratrol fermentation liquor according to claim 1 is characterized in that the crystallization treatment process comprises the steps of cooling the concentrated liquor to 4-8 ℃ for crystallization to obtain resveratrol crude product, mixing and dissolving the resveratrol crude product and ethanol to obtain a dissolution liquor, adding water into the dissolution liquor, and recrystallizing at the temperature of 25-30 ℃ to obtain resveratrol.

Description

Separation method of resveratrol fermentation liquor Technical Field The invention relates to the field of purification and preparation of resveratrol, in particular to a separation method of resveratrol fermentation liquor. Background Resveratrol is a non-flavonoid polyphenol compound, also called as stilbene trisol, and has a molecular formula of C 14H12O3. Resveratrol is a natural antioxidant, and has effects in reducing blood viscosity, inhibiting blood platelet coagulation and vasodilation, keeping blood smooth, scavenging active oxygen such as superoxide anion and hydroxyl radical, inhibiting lipid peroxidation, and reducing cell injury caused by oxidative stress. Resveratrol has antiinflammatory effect, and can inhibit release of inflammatory factors such as TNF-alpha and IL-6, down regulate inflammatory signal pathway such as NF- κB, and relieve arthritis and intestinal tract inflammation in animal model. In addition, resveratrol has tumor inhibiting effect, and can be used for treating diseases such as breast cancer. Resveratrol is widely applied to the fields of medicines, foods and the like, for example, in the medicine field, resveratrol can be applied to the aspects of resisting tumors, reducing blood sugar, protecting nerves and the like, and in the food field, resveratrol is listed in the examination and approval catalogue of new food raw materials in 2023 and can be applied to foods such as functional beverages, health bars and the like. The production technology of resveratrol mainly comprises three main routes of plant extraction, chemical synthesis and biological synthesis, wherein the biological synthesis technology has more application potential, and the fermentation liquor containing resveratrol is usually produced by fermenting raw materials such as giant knotweed by microorganisms, and then the resveratrol is extracted from the fermentation liquor. At present, the purification method of resveratrol in the industrial fermentation liquor is generally macroporous resin, silica gel or ion exchange resin chromatography, but the methods have long period, high cost, low purity and low yield and need to be solved. Disclosure of Invention The invention provides a separation method of resveratrol fermentation liquor, which can shorten the extraction period of resveratrol, reduce the cost and improve the purity and the yield of resveratrol under the condition of not using a chromatographic method. In one aspect of the invention, a method for separating resveratrol fermentation broth is provided, which comprises the following steps: (1) Carrying out filter pressing treatment on resveratrol fermentation liquor to obtain second filter residues; wherein, the filter pressing treatment of resveratrol fermentation liquor comprises a first treatment or a second treatment: the first treatment process comprises the steps of adjusting the pH value of resveratrol fermentation liquor to be acidic, and then carrying out first filter pressing to obtain first filter residues; the second treatment process comprises the steps of adjusting the pH value of resveratrol fermentation liquor to be alkaline, and then carrying out third filter pressing to obtain first filter residues; (2) Extracting the second filter residue by adopting an organic solvent to obtain an extract containing resveratrol; (3) Washing the extract liquid to obtain a washing liquid containing resveratrol, wherein the washing treatment comprises sequentially performing alkali washing treatment and acid washing treatment on the extract liquid to obtain a washing liquid containing resveratrol, or sequentially performing acid washing treatment and alkali washing treatment on the extract liquid to obtain a washing liquid containing resveratrol; (4) Dewatering and decoloring the washing liquid containing resveratrol, and concentrating to obtain concentrated liquid; (5) And (3) crystallizing the concentrated solution to obtain resveratrol. According to one embodiment of the invention, the pH value of the resveratrol fermentation liquor is regulated to be acidic in the first treatment process, specifically, the pH value of the resveratrol fermentation liquor is regulated to be 2-4, and/or the pH value of the resveratrol fermentation liquor is regulated to be acidic by adopting inorganic acid in the first treatment process, wherein the inorganic acid comprises one or more of hydrochloric acid, oxalic acid, acetic acid, sulfuric acid and phosphoric acid, and/or the first filter pressing is plate-frame filter pressing. According to one embodiment of the invention, the first alkali liquor comprises an ammonium bicarbonate aqueous solution, the mass concentration of ammonium bicarbonate in the ammonium bicarbonate aqueous solution is 5% -6%, the ratio of the volume of the ammonium bicarbonate aqueous solution to the mass of the first filter residue is (1-2) L:1Kg, and/or the first mixing treatment is carried out in a stirring state, the time of the first mix