CN107162888A - The production method of resveratrol and rheum emodin is prepared from giant knotweed - Google Patents

The production method of resveratrol and rheum emodin is prepared from giant knotweed Download PDF

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Publication number
CN107162888A
CN107162888A CN201710396578.7A CN201710396578A CN107162888A CN 107162888 A CN107162888 A CN 107162888A CN 201710396578 A CN201710396578 A CN 201710396578A CN 107162888 A CN107162888 A CN 107162888A
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resveratrol
giant knotweed
ethanol
crude product
rheum emodin
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CN201710396578.7A
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吴世华
叶艳
罗祥
马松
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Hubei Zhongxin Biotech Co Ltd
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Hubei Zhongxin Biotech Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C46/00Preparation of quinones
    • C07C46/10Separation; Purification; Stabilisation; Use of additives
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00Preparation of oxygen-containing organic compounds
    • C12P7/02Preparation of oxygen-containing organic compounds containing a hydroxy group
    • C12P7/22Preparation of oxygen-containing organic compounds containing a hydroxy group aromatic

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  • Organic Chemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Zoology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Microbiology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Biotechnology (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Cosmetics (AREA)

Abstract

The invention provides the production method that resveratrol and rheum emodin are prepared from giant knotweed, the crushing of giant knotweed stem tuber will be dried and be screened to 10 30 mesh, by 0.5 0.8 times of giant knotweed quality after the crushing wettings that add water, yeast is added, fermented 48 72 hours at 45 DEG C~50 DEG C;Then ethanol extraction, concentration, upper prop, elution, concentration, crystallization, dry resveratrol crude product are added;Resveratrol crude product is recrystallized to give the resveratrol of high-purity.The technical process of the present invention is safe, economical, easy to operate, and is easily achieved the resveratrol that the large-scale production from giant knotweed prepares high-purity.

Description

The production method of resveratrol and rheum emodin is prepared from giant knotweed
Technical field
Field is extracted the present invention relates to plant functional component, is specifically that one kind prepares resveratrol and rheum emodin from giant knotweed Production method.
Background technology
Resveratrol is called the another new green cancer therapy drug after taxol, have it is significant suppress cancer cell, Reduce the effect such as blood fat, prevention and cure of cardiovascular disease, anti-oxidant, strengthen immunity, anti-aging.Pharmacy, food, health products and Have and be widely applied in the industries such as cosmetics.In recent years, the health food using resveratrol as active component emerges in an endless stream: Resveratrol(Also known as resvertrol), chemistry entitled 3,4,5 ,-trihydroxy talan(3,4,5 ,- trihydrolystilbene), it is the non-flavones polyphenol compound containing stilbene class formation.Resveratrol is plant by should A kind of antitoxin of itself synthesis when swashing, with important smooth activity.Hydroxyl is rich in resveratrol molecule structure, with catching Obtaining the hexichol alkene structure in free radical, oxidation resistance, its molecule has the ability for absorbing ultraviolet light, and these characteristics are by cosmetic conduct Industry is fully applied.Resveratrol is all distributed in many plants, but polygonaceae plant Resveratrol in Rhizoma Polygoni Cuspidati content is highest, It is the most preferable resource for obtaining natural resveratrol up to 0.1-0.4%.In view of resveratrol is in medicine, health products, cosmetics city Field, which has, to be increasingly widely applied, and structure is simple to operate, with low cost, it is easy to which the separation that high-volume obtains resveratrol sterling is pure Change technology, has wide practical use and significance.
The content of the invention
A kind of preparation from giant knotweed it is an object of the invention to provide low cost, without toxic solvent, energy industrialized production The production method of resveratrol and rheum emodin.
The technical solution adopted by the present invention is:The production method of resveratrol and rheum emodin is prepared from giant knotweed, its feature It is, comprises the following steps:
(1)Giant knotweed is crushed, 10-30 mesh powder is obtained;
(2)By the giant knotweed quality after crushing, the water for adding 0.5-0.8 times soaks, adds the yeast of 9-10 ‰, be placed in fermentation tank, Fermented 48-72 hours at a temperature of 45 DEG C~50 DEG C, polygonin is changed into resveratrol;
(3)By the giant knotweed quality after crushing, the ethanol of 10-14 times of addition, refluxing extraction at least 2 times;Wherein, ethanol is 60-70% Ethanol;
(4)Extract solution is merged, filtered, concentration and recovery ethanol obtains extraction medicinal extract;2-3 times of quality of addition in medicinal extract is extracted Water sedimentation, centrifuge, filter residue and centrifugate;Filter residue and drying is product rheum emodin;
(5)Macroporous absorbent resin in centrifugate, is eluted to colourless with pure water, then with 2BV 25% ethanol elution, is discarded; 1.5BV 80% ethanol elution is finally used, 1.5BV eluent is collected;
(6)By the eluent being collected into concentration, dry, obtain resveratrol crude product;
(7)Resveratrol crude product is recrystallized:Resveratrol crude product is dissolved with 80% ethanol, be configured to solid content for 10% it is molten Liquid, added by crude product resveratrol weight 3 ‰ activated carbon, 55-65 DEG C of decolouring 1-1.5 hours, centrifugal filtration, filtrate is concentrated into Solid content 50%, obtains medicinal extract;95% ethanol of medicinal extract quality 20% is added, recrystallization is placed 12-48 hours, refiltered, finally will knot Crystalline substance vacuum drying produces resveratrol.
Further restriction to above-mentioned technical proposal:The macroporous absorbent resin is LS101 resins or LX-17 resins.
The device have the advantages that:
1st, the present invention is using the method for alcohol extracting-water precipitating, and production cost is low, while obtaining byproduct rheum emodin;
2nd, it is with short production cycle, water and ethanol are only used in production, without other organic solvent safety and environmental protections;
3rd, resveratrol product purity >=98%.
Embodiment
Embodiment 1
Rhizoma Polygoni Cuspidati is dried and crushed into giant knotweed powder, 10-30 mesh sieves are crossed, giant knotweed powder 1000Kg, plus the wetting of 700KG water is taken;Will 9.6Kg yeast is added in 100KG water, adjusts pH=4.5, is then added and is stirred in giant knotweed, 50 DEG C of fermentation 72h.Add 70% Alcohol reflux is extracted twice, and filtering merges extract solution, solid content 20% is concentrated into, after 2 times of water of addition medicinal extract amount are sufficiently stirred for Centrifugation, obtains filter residue and centrifugate.Filter residue is washed with water rear heated-air drying and obtains rheum emodin.Extracting centrifugal liquid, upper LS101 resins, pure water It is washed till colourless, then with 20% ethanol elution 2BV, finally uses 80% ethanol elution, collects 1.5BV eluents, it is eluent concentration, dry Dry, HPLC is determined, and obtains the resveratrol crude product of purity 62.7%.
Embodiment 2
Rhizoma Polygoni Cuspidati is dried and crushed into giant knotweed powder, 10-30 mesh sieves are crossed, giant knotweed powder 1000Kg, plus the wetting of 700KG water is taken;Will 9.6Kg yeast is added in 100KG water, adjusts pH=4.5, is then added and is stirred in giant knotweed, 50 DEG C of fermentation 72h.Add 70% Alcohol reflux is extracted twice, and filtering merges extract solution, solid content 20% is concentrated into, after 2 times of water of addition medicinal extract amount are sufficiently stirred for Centrifugation, obtains filter residue and centrifugate.Filter residue is washed with water rear heated-air drying and obtains rheum emodin.Extracting centrifugal liquid, upper LX-17 resins, pure water It is washed till colourless, then with 20% ethanol elution 2BV, finally uses 80% ethanol elution, collects 1.5BV eluents, it is eluent concentration, dry Dry, HPLC is determined, and obtains the resveratrol crude product of purity 63.3%.
Embodiment 3
Rhizoma Polygoni Cuspidati is dried and crushed into giant knotweed powder, 10-30 mesh sieves are crossed, giant knotweed powder 1000Kg, plus the wetting of 700KG water is taken;Will 9.6Kg yeast is added in 100KG water, adjusts pH=4.5, is then added and is stirred in giant knotweed, 50 DEG C of fermentation 72h.Add 70% Alcohol reflux is extracted twice, and filtering merges extract solution, solid content 20% is concentrated into, after 2 times of water of addition medicinal extract amount are sufficiently stirred for Centrifugation, obtains filter residue and centrifugate.Filter residue is washed with water rear heated-air drying and obtains rheum emodin.Extracting centrifugal liquid, upper LS101 resins, pure water It is washed till colourless, then with 25% ethanol elution 2BV, finally uses 80% ethanol elution, collects 1.5BV eluents, it is eluent concentration, dry Dry, HPLC is determined, and obtains the resveratrol crude product of purity 65.4%.
Embodiment 4
Rhizoma Polygoni Cuspidati is dried and crushed into giant knotweed powder, 10-30 mesh sieves are crossed, giant knotweed powder 1000Kg, plus the wetting of 700KG water is taken;Will 9.6Kg yeast is added in 100KG water, adjusts pH=4.5, is then added and is stirred in giant knotweed, 50 DEG C of fermentation 72h.Add 70% Alcohol reflux is extracted twice, and filtering merges extract solution, solid content 20% is concentrated into, after 2 times of water of addition medicinal extract amount are sufficiently stirred for Centrifugation, obtains filter residue and centrifugate.Filter residue is washed with water rear heated-air drying and obtains rheum emodin.Extracting centrifugal liquid, upper LX-17 resins, pure water It is washed till colourless, then with 25% ethanol elution 2BV, finally uses 80% ethanol elution, collects 1.5BV eluents, it is eluent concentration, dry Dry, HPLC is determined, and obtains the resveratrol crude product of purity 68.7%.
Embodiment 5
Resveratrol is recrystallized:The resveratrol crude product product that embodiment 1 or embodiment 2 or embodiment 3 or embodiment 4 are produced are used 80% ethanol is dissolved, and is configured to the solution that solid content is 10%, and 3 ‰ activated carbon, 55-65 DEG C are added by crude product resveratrol weight Decolouring 1-1.5 hours, centrifugal filtration, filtrate is concentrated into solid content 50%, obtains medicinal extract;95% ethanol of medicinal extract quality 20% is added, is put Put recrystallization 12-48 hours, refilter, will finally crystallize and be dried in vacuo the resveratrol for producing purity >=98%.

Claims (2)

1. the production method of resveratrol and rheum emodin is prepared from giant knotweed, it is characterised in that comprise the following steps:
(1)Giant knotweed is crushed, 10-30 mesh powder is obtained;
(2)By the giant knotweed quality after crushing, the water for adding 0.5-0.8 times soaks, adds the yeast of 9-10 ‰, be placed in fermentation tank, Fermented 48-72 hours at a temperature of 45 DEG C~50 DEG C, polygonin is changed into resveratrol;
(3)By the giant knotweed quality after crushing, the ethanol of 10-14 times of addition, refluxing extraction at least 2 times;Wherein, ethanol is 60-70% Ethanol;
(4)Extract solution is merged, filtered, concentration and recovery ethanol obtains extraction medicinal extract;2-3 times of quality of addition in medicinal extract is extracted Water sedimentation, centrifuge, filter residue and centrifugate;Filter residue and drying is product rheum emodin;
(5)Macroporous absorbent resin in centrifugate, is eluted to colourless with pure water, then with 2BV 25% ethanol elution, is discarded; 1.5BV 80% ethanol elution is finally used, 1.5BV eluent is collected;
(6)By the eluent being collected into concentration, dry, obtain resveratrol crude product;
(7)Resveratrol crude product is recrystallized:Resveratrol crude product is dissolved with 80% ethanol, be configured to solid content for 10% it is molten Liquid, added by crude product resveratrol weight 3 ‰ activated carbon, 55-65 DEG C of decolouring 1-1.5 hours, centrifugal filtration, filtrate is concentrated into Solid content 50%, obtains medicinal extract;95% ethanol of medicinal extract quality 20% is added, recrystallization is placed 12-48 hours, refiltered, finally will knot Crystalline substance vacuum drying produces resveratrol.
2. the production method according to claim 1 that resveratrol and rheum emodin are prepared from giant knotweed, it is characterised in that institute Macroporous absorbent resin is stated for LS101 resins or LX-17 resins.
CN201710396578.7A 2017-05-31 2017-05-31 The production method of resveratrol and rheum emodin is prepared from giant knotweed Pending CN107162888A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101698634A (en) * 2009-06-30 2010-04-28 三原润禾植化有限公司 Method for extracting and separating resveratrol from giant knotweed rhizome
CN101792373A (en) * 2010-03-18 2010-08-04 重庆科瑞南海制药有限责任公司 Process for extracting, separating and purifying high-purity resveratrol
CN102219652A (en) * 2011-05-05 2011-10-19 三明华健生物工程有限公司 Method for preparing water-soluble resveratrol from giant knotweed rhizome
CN102838456A (en) * 2012-09-17 2012-12-26 湖南希尔天然药业有限公司 Technology for preparing resveratrol by using traditional Chinese medicine giant knotweed rhizome
CN102838455A (en) * 2012-09-17 2012-12-26 湖南希尔天然药业有限公司 Method for extracting high-content resveratrol from polygonum cuspidatum
CN104263763A (en) * 2014-09-04 2015-01-07 南京标科生物科技有限公司 Novel method for extracting resveratrol from giant knotweed
CN104341277A (en) * 2014-11-18 2015-02-11 白心亮 Method for extracting resveratrol from Polygonum cuspidatum

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101698634A (en) * 2009-06-30 2010-04-28 三原润禾植化有限公司 Method for extracting and separating resveratrol from giant knotweed rhizome
CN101792373A (en) * 2010-03-18 2010-08-04 重庆科瑞南海制药有限责任公司 Process for extracting, separating and purifying high-purity resveratrol
CN102219652A (en) * 2011-05-05 2011-10-19 三明华健生物工程有限公司 Method for preparing water-soluble resveratrol from giant knotweed rhizome
CN102838456A (en) * 2012-09-17 2012-12-26 湖南希尔天然药业有限公司 Technology for preparing resveratrol by using traditional Chinese medicine giant knotweed rhizome
CN102838455A (en) * 2012-09-17 2012-12-26 湖南希尔天然药业有限公司 Method for extracting high-content resveratrol from polygonum cuspidatum
CN104263763A (en) * 2014-09-04 2015-01-07 南京标科生物科技有限公司 Novel method for extracting resveratrol from giant knotweed
CN104341277A (en) * 2014-11-18 2015-02-11 白心亮 Method for extracting resveratrol from Polygonum cuspidatum

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Title
刘丹等: ""大孔吸附树脂吸附纯化虎杖有效部位的研究"", 《中国中药杂志》 *

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