Method for preparing fisetin by enzyme method

A technology of enzymatic preparation and fisetin, applied in organic chemistry and other directions, can solve problems such as poor bioavailability and stability, achieve good bioavailability and stability, avoid organic solvent reflux extraction, and high extraction rate of raw materials. Effect

Pending Publication Date: 2021-12-07
雅安职业技术学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, the color of needle-like crystals is closer to the true color of fisetin, with better bioavailability and stability, and the color of powdered crystals is deeper, which is different from the natural color of fisetin, with better bioavailability and stability worse than acicular crystals

Method used

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  • Method for preparing fisetin by enzyme method
  • Method for preparing fisetin by enzyme method
  • Method for preparing fisetin by enzyme method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] A method for enzymatically preparing fisetin, comprising the following steps:

[0062] Step (1) enzymatic hydrolysis:

[0063] Grind the raw material sumac, take 200g raw material, add 2000ml citric acid solution, adjust the pH value to 5, add 2g plant extract complex enzyme, stir at 50°C for 4 hours, so that fisetin can be fully dissolved into the citric acid solution; Extract complex enzymes from living plants, collect the enzymatic solution; repeat the enzymatic extraction of raw materials, and combine the enzymatic solution to 3650ml;

[0064] Step (2) crude:

[0065] Concentrate the combined enzymolysis solution into 26.9g of extract, add 450ml of 95% methanol to the extract, heat until completely dissolved, then cool to room temperature and filter, the filtrate is concentrated, crystallized and dried to obtain 6.4g of crude fisetin ;

[0066] Step (3) recrystallization refinement:

[0067] 6.4g of crude fisetin was recrystallized twice using a recrystallizatio...

Embodiment 2

[0070] Grind the sumac raw material, weigh 200g raw material and put it into a three-neck flask, add 2000ml pH=5 citric acid solution, add 2.5g plant extract complex enzyme, stir at 50°C for 4 hours, add 5% NaoH solution to adjust pH=7 , collect the enzymolysis solution; repeat the above steps to combine the enzymolysis solution to a total of 3700ml.

[0071] 2) Concentrate the enzymatic solution in vacuum to obtain 31g of extract;

[0072] 3) Add 460ml of methanol with a purity of 99% to the extract, heat to dissolve completely, cool to room temperature, filter, concentrate, crystallize and dry the filtrate to obtain 6.1g of crude fisetin.

[0073] 4) Repeat the crystallization of 6.1g of crude fisetin twice twice to obtain 2.3g of fisetin. The first recrystallization uses 192ml of 1:1 acetone / ethanol mixture, and the second recrystallization uses 192ml of 98% methanol.

[0074] The HPLC detection normalization method content was 98.7%, and the external standard method conte...

Embodiment 3

[0076] Grind the raw material of sumac, weigh 50kg of raw material in the extraction tank, add 350kg of water, add citric acid solution to adjust pH = 5, add 500g of plant extraction complex enzyme, cycle at 50°C for 4 hours, heat to boiling and return for 1 hour , collect the enzymolysis solution; repeat the above steps to combine the enzymolysis solution to a total of 630L.

[0077] 2) Concentrate the enzymatic solution in vacuum to obtain 7kg of extract;

[0078] 3) Add 70kg of 95% ethanol to the extract, heat to dissolve completely, cool to room temperature, filter, concentrate, crystallize and dry the filtrate to obtain 1.3kg of crude fisetin.

[0079] 4) Recrystallize 1.3kg of crude fisetin twice to obtain 505g of fisetin. The first recrystallization uses 192ml of 98% acetone / 95% ethanol mixture of 1:1, and the second recrystallization uses 192ml of 98% methanol .

[0080] The content of HPLC was 98.1% by normalization method and 97.6% by external standard method; the ...

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Abstract

The invention discloses a method for preparing fisetin by an enzyme method. The method comprises the steps: crushing a raw material cotinus coggygria, and adding a citric acid solution and a plant extraction compound enzyme so as to enable the fisetin to be fully dissolved out of the citric acid solution; collecting enzymatic hydrolysate; concentrating the combined enzymatic hydrolysate into extract, adding high alcohol into the extract until the high alcohol is completely dissolved, and concentrating, crystallizing and drying filtrate to obtain a fisetin crude product; and recrystallizing the fisetin crude product twice by using a recrystallization solvent to obtain a high-purity fisetin refined product after twice recrystallization. According to the method, the citric acid solution is adopted to extract fisetin, so that fat-soluble substances in the enzymatic hydrolysate are extremely few, refining can be directly completed through a recrystallization process, a column chromatography process is not needed, the process operation difficulty and efficiency are reduced, the production efficiency is improved, and the method is suitable for industrial production. According to the invention, the recrystallization process is optimized, so that the refined fisetin product obtained after recrystallization is a needle-like crystal.

Description

technical field [0001] The invention relates to the technical field of extraction of active ingredients of traditional Chinese medicines, in particular to a method for preparing fisetin by an enzymatic method. Background technique [0002] Sumac (Cotinus coggygria Scop.), a plant of the genus Sumac in the Anacardaceae family, is an important ornamental red-leaved tree species. Its roots and stems can be used as medicine for the treatment of jaundice hepatitis and chronic hepatitis. Pharmacological experiments have shown that the active ingredients in cotinus sumac are mainly flavonoids, especially fisetin; the content of fisetin in cotinus cotinus is about 2%. Fisetin is a yellow-like substance, and its molecular structure is as follows: [0003] . [0004] From the chemical structural formula of fisetin, it can be seen that 3-OH exists, and fisetin belongs to flavonols in flavonoids, all atoms in the molecule are in the same plane, and exist in the xylem of sumac suma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/30C07D311/40
CPCC07D311/30C07D311/40
Inventor 梁林辉杜翠华梁大伟
Owner 雅安职业技术学院
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