CN106214731A - Blueberry raw anthocyanidin biological extraction process - Google Patents

Blueberry raw anthocyanidin biological extraction process Download PDF

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Publication number
CN106214731A
CN106214731A CN201610762644.3A CN201610762644A CN106214731A CN 106214731 A CN106214731 A CN 106214731A CN 201610762644 A CN201610762644 A CN 201610762644A CN 106214731 A CN106214731 A CN 106214731A
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filtrate
extraction process
biological extraction
blueberry raw
extract
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许华礼
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Shenli Blueberry Group Co Ltd
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Shenli Blueberry Group Co Ltd
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Priority to CN201610762644.3A priority Critical patent/CN106214731A/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/45Ericaceae or Vacciniaceae (Heath or Blueberry family), e.g. blueberry, cranberry or bilberry
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/55Liquid-liquid separation; Phase separation

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The present invention relates to technical field of biological extraction, be specifically related to a kind of blueberry raw anthocyanidin biological extraction process.Blueberry raw anthocyanidin biological extraction process, step is: mixed with blue berry berry marc powder by acidic ethanol, heating and refluxing extraction, filter and collect filtrate and residue, residue mixes with the acidic ethanol solution of identical solid-liquid ratio with same concentration again, reflux, extract, again, filters and collects filtrate, merges the filtrate of twice;Filtrate low temperature is placed, then filters, concentration is evaporated under reduced pressure;Then pass through microporous filter membrane and carry out hyperfiltration treatment, to remove antibacterial and high molecular weight protein;Finally by column chromatography purification, drying and other steps.The present invention proposes the biological extraction process of a kind of blueberry raw anthocyanidin, and the method, according to different product categories, can extract the procyanidin that purity is 25~51%, and this technology is current domestic state-of-the-art blueberry raw anthocyanidin extractive technique.And, compared with external similar technique, also there is lower-cost advantage.

Description

Blueberry raw anthocyanidin biological extraction process
Technical field
The present invention relates to technical field of biological extraction, be specifically related to a kind of blueberry raw anthocyanidin biological extraction process.
Background technology
Containing abundant procyanidin nutritional labeling in Blueberry, procyanidin not only has good nourishing healthy and makees With, also have and prevent that cranial nerve is aging, heart tonifying, anticancer vessel softening, strengthen the functions such as human organism's immunity.Effect of procyanidin Value expression exists:
(1) antioxidation and removing free radical: OPC are owing to there being the hydroxylic moiety of electron rich in its molecular structure, are excellent Hydrogen or the donor of neutron, therefore have superpower oxidation resistance, can effectively remove the free radical in human body.Procyanidin exists Vivo and vitro has antioxidant activity.
(2) protection cardio-cerebrovascular: procyanidin is obvious to the protective effect of cerebral ischemia reperfusion injury;People can be suppressed The propagation of class skin capillary endothelial cell, affects angiogenesis;Having clear and definite antiplatelet aggregative activity, antithrombotic is made With substantially;Reduce plasma triglyceride free fatty apolipoprotein B, improve Atherosclerosis Risk index after the meal;Have Stronger adjustment blood fat, promotes reverse cholesterol transport and accelerates lipid and Cholesterol Excretion, improving the effect of lipid metabolic disorder.
(3) anti-curing cancers: procyanidin has antitumor action, to cervical cancer, many cancers such as carcinoma of prostate, colon cancer There are prevention and the effect for the treatment of.Additionally, the cancers such as skin carcinoma, oral cancer, hepatocarcinoma are still had certain effect by procyanidin.
(4) prevent with treatment diabetes: procyanidin can improve the oxidised form of diabetic disease states, to insulin sensitivity The ILA of cell line and antioxidant activity.
(5) antiinflammatory action: procyanidin as antiinflammatory, thus plays antiinflammatory in the macrophage that endotoxin stimulates Effect.
(6) gastric ulcer injury protection effect: procyanidin can suppress the generation of stress gastric ulcer, suppression gastric mucosa Secretion acid function, reduces pepsic activity simultaneously.
(7) the liver protecting effect: low dose of (50,100mg L-1) procyanidin can suppress ethanol and tetrachloro-methane induction Hepatocyte injury and stimulate normal liver cell propagation.
(8) radiation resistance: procyanidin can reduce the Fas protein expression integration of roentgenization skin, increases Bc1-2 Protein expression integration, is allowed to close to normal skin.
(9) enzyme inhibition: procyanidin has inhibitory action to multiple enzyme, it can effectively suppress external pancreatic lipase Activity, its effect with the degree of polymerization increase and strengthen.
(10) other effects: procyanidin also has mutation, antiallergic, anti HIV-1 virus, antidepressant, antifatigue effect, Treatment acute respiratory distress syndrome, delays the decline of audition, promotes hair growth and analgesic activity.
At present, blueberry raw anthocyanidin carrying out separation and Extraction and deep processing is always industrial hot spot, external Producer is existing Utilizing the research that blueberry raw anthocyanidin pharmacy, fine chemical product research and development etc. are relevant, this measure can be substantially improved value of the product and profit Profit return rate, widens the development space of blueberry industry simultaneously.
Summary of the invention
For technical problem present in prior art, it is an object of the invention to provide a kind of blueberry raw anthocyanidin biological Extracting method, to achieve these goals, the technical solution adopted in the present invention is:
A kind of blueberry raw anthocyanidin biological extraction process, step is as follows:
1) extract: by concentration be 35~75%, pH value be ethanol and the blue berry berry marc powder of 2.5~5.5 with 3~9: 1 part by weight mixing, heating and refluxing extraction 1~2h, filter and collect filtrate and residue, residue again with identical solid-liquid ratio with Mix with the acidic ethanol solution of concentration, reflux, extract, 1~2h again, filter and collect filtrate, merge the filtrate of twice;
2) remove impurity: by step 1) gained merging filtrate 0~4 DEG C of low temperature put 15~20h, then filter;
3) concentrate: by step 2) gained filtrate is evaporated under reduced pressure at 55 DEG C concentrate 10~12h;
4) ultrafiltration: by step 3) gained concentrated solution surpassed by microporous filter membrane (aperture may select 0.40um and 0.20um) Filter processes, to remove antibacterial and high molecular weight protein;
5) column chromatography purification: first filtrate is flow through macroporous adsorbent resin, then with the speed of per hour 1~3 times of column volume Flow through resin with the distilled water of 2~5 times of column volumes with identical speed, wash away major part impurity, then with the 60 of 1~3 column volumes ~the ethanol solution of 90% flows through resin with identical speed, the anthocyanin that resin adsorbs is eluted, collect eluent;
6) it is dried: eluent is evaporated under reduced pressure at 55 DEG C concentration and removes ethanol further, finally in 40~55 DEG C of vacuum Environment is dried.
The blueberry raw anthocyanidin biological extraction process of the present invention, its beneficial effect shows:
The present invention proposes the biological extraction process of a kind of blueberry raw anthocyanidin, the method according to different product categories, Can extract the procyanidin that purity is 25~51%, this technology is that current domestic state-of-the-art blueberry raw anthocyanidin extracts skill Art.And, compared with external similar technique, also there is lower-cost advantage.
Accompanying drawing explanation
Fig. 1 is the flow chart of the blueberry raw anthocyanidin biological extraction process of the present invention.
Detailed description of the invention
For further describing the blueberry raw anthocyanidin biological extraction process of the present invention, below in conjunction with the accompanying drawings it is made further Explanation.
Embodiment 1
Referring to Fig. 1, a kind of blueberry raw anthocyanidin biological extraction process, step is as follows:
1) extract: by concentration be 60%, pH value be that ethanol and the blue berry berry marc powder of 4.5 are with the part by weight of 5:1 Mixing, heating and refluxing extraction 1.5h, filter and collect filtrate and residue, residue is again with identical solid-liquid ratio and the acidifying with concentration Ethanol solution mixes, and reflux, extract, 1.5h again filters and collects filtrate, merges the filtrate of twice.
2) remove impurity: by step 1) 2 DEG C of low temperature of gained merging filtrate put 18h, then filter.
3) concentrate: by step 2) gained filtrate is evaporated under reduced pressure at 55 DEG C concentrate 11h.
4) ultrafiltration: by step 3) gained concentrated solution carries out hyperfiltration treatment by microporous filter membrane, to remove antibacterial and macromole Albumen.
5) column chromatography purification: first filtrate is flow through macroporous adsorbent resin with the speed of per hour 2 times of column volumes, then with 3 The distilled water of times column volume flows through resin with identical speed, washes away major part impurity, then the ethanol with the 70% of 1 column volume is molten Liquid flows through resin with identical speed, is eluted by the anthocyanin that resin adsorbs, and collects eluent.
6) it is dried: eluent is evaporated under reduced pressure at 55 DEG C concentration and removes ethanol further, finally 50 DEG C of vacuum environments In be dried, obtain blueberry raw anthocyanidin, in extract, anthocyanin content is 48%.
Embodiment 2
A kind of blueberry raw anthocyanidin biological extraction process, step is as follows:
1) extract: by concentration be 70%, pH value be 3 ethanol mix with the part by weight of 8:1 with blue berry berry marc powder Closing, heating and refluxing extraction 1.2h, filter and collect filtrate and residue, residue is again with identical solid-liquid ratio and the acidifying second with concentration Alcoholic solution mixes, and reflux, extract, 1.2h again filters and collects filtrate, merges the filtrate of twice.
2) remove impurity: by step 1) 3 DEG C of low temperature of gained merging filtrate put 16h, then filter.
3) concentrate: by step 2) gained filtrate is evaporated under reduced pressure at 55 DEG C concentrate 12h.
4) ultrafiltration: by step 3) gained concentrated solution carries out hyperfiltration treatment by microporous filter membrane, to remove antibacterial and macromole Albumen.
5) column chromatography purification: first filtrate is flow through macroporous adsorbent resin with the speed of per hour 1 times of column volume, then with 5 The distilled water of times column volume flows through resin with identical speed, washes away major part impurity, then the ethanol with the 80% of 1 column volume is molten Liquid flows through resin with identical speed, is eluted by the anthocyanin that resin adsorbs, and collects eluent.
6) it is dried: eluent is evaporated under reduced pressure at 55 DEG C concentration and removes ethanol further, finally 45 DEG C of vacuum environments In be dried, obtain blueberry raw anthocyanidin, in extract, anthocyanin content is 35%.
Embodiment 3
A kind of blueberry raw anthocyanidin biological extraction process, step is as follows:
1) extract: by concentration be 40%, pH value be 5 ethanol mix with the part by weight of 4:1 with blue berry berry marc powder Closing, heating and refluxing extraction 2h, filter and collect filtrate and residue, residue is again with identical solid-liquid ratio and the acidic ethanol with concentration Solution mixes, and reflux, extract, 2h again filters and collects filtrate, merges the filtrate of twice.
2) remove impurity: by step 1) 1 DEG C of low temperature of gained merging filtrate puts 19h, then filters.
3) concentrate: by step 2) gained filtrate is evaporated under reduced pressure at 55 DEG C concentrate 10h.
4) ultrafiltration: by step 3) gained concentrated solution carries out hyperfiltration treatment by microporous filter membrane, to remove antibacterial and macromole Albumen.
5) column chromatography purification: first filtrate is flow through macroporous adsorbent resin with the speed of per hour 3 times of column volumes, then with 2 The distilled water of times column volume flows through resin with identical speed, washes away major part impurity, then the ethanol with the 65% of 3 column volumes is molten Liquid flows through resin with identical speed, is eluted by the anthocyanin that resin adsorbs, and collects eluent.
6) it is dried: eluent is evaporated under reduced pressure at 55 DEG C concentration and removes ethanol further, finally in 40~55 DEG C of vacuum Being dried in environment, obtain blueberry raw anthocyanidin, in extract, anthocyanin content is 38%.
Above content is only the design example to the present invention and explanation, affiliated those skilled in the art Described specific embodiment is made various amendment or supplements or use similar mode to substitute, without departing from invention Design or surmount scope defined in the claims, protection scope of the present invention all should be belonged to.

Claims (1)

1. a blueberry raw anthocyanidin biological extraction process, it is characterised in that step is as follows:
1) extract: by concentration be 35~75%, pH value be that ethanol and the blue berry berry marc powder of 2.5~5.5 are with 3~9:1 Part by weight mix, heating and refluxing extraction 1~2h, filter and collect filtrate and residue, residue again with identical solid-liquid ratio with The acidic ethanol solution mixing of concentration, reflux, extract, 1~2h again, filter and collect filtrate, merge the filtrate of twice;
2) remove impurity: by step 1) gained merging filtrate 0~4 DEG C of low temperature put 15~20h, then filter;
3) concentrate: by step 2) gained filtrate is evaporated under reduced pressure at 55 DEG C concentrate 10~12h;
4) ultrafiltration: by step 3) gained concentrated solution carries out hyperfiltration treatment by microporous filter membrane, to remove antibacterial and high molecular weight protein;
5) column chromatography purification: first filtrate is flow through macroporous adsorbent resin with the speed of per hour 1~3 times of column volume, then with 2~ The distilled water of 5 times of column volumes flows through resin with identical speed, washes away major part impurity, then with the 60~90% of 1~3 column volumes Ethanol solution flow through resin with identical speed, the anthocyanin that resin adsorbs is eluted, collect eluent;
6) it is dried: eluent is evaporated under reduced pressure at 55 DEG C concentration and removes ethanol further, finally 40~55 DEG C of vacuum environments In be dried.
CN201610762644.3A 2016-08-29 2016-08-29 Blueberry raw anthocyanidin biological extraction process Pending CN106214731A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109096236A (en) * 2018-08-13 2018-12-28 安徽兆龙生物科技有限公司 Blueberry procyanidine biological extraction process
CN112778260A (en) * 2020-12-31 2021-05-11 齐鲁工业大学 Blueberry anthocyanin-rich extract and preparation method thereof

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CN103289430A (en) * 2013-06-27 2013-09-11 安徽省林锦记食品工业有限公司 Method for extracting and purifying anthocyanins from blueberry pomaces

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CN101525325A (en) * 2008-03-06 2009-09-09 陕西嘉禾植物化工有限责任公司 Method for extracting anthocyanin from cowberry
CN101265252A (en) * 2008-04-28 2008-09-17 吉林大学 Vaccinium uliginosum cyanidin and separation and purification method thereof
CN103289430A (en) * 2013-06-27 2013-09-11 安徽省林锦记食品工业有限公司 Method for extracting and purifying anthocyanins from blueberry pomaces

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109096236A (en) * 2018-08-13 2018-12-28 安徽兆龙生物科技有限公司 Blueberry procyanidine biological extraction process
CN112778260A (en) * 2020-12-31 2021-05-11 齐鲁工业大学 Blueberry anthocyanin-rich extract and preparation method thereof

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