CN107281252A - A kind of preparation method of whortle extract - Google Patents

A kind of preparation method of whortle extract Download PDF

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CN107281252A
CN107281252A CN201710522268.5A CN201710522268A CN107281252A CN 107281252 A CN107281252 A CN 107281252A CN 201710522268 A CN201710522268 A CN 201710522268A CN 107281252 A CN107281252 A CN 107281252A
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extract
whortle
preparation
solution
extracted
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CN107281252B (en
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季亚飞
周凯
冯定军
刘帮民
梁岩
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Yangling Kin Kin Bioengineering Technology Co Ltd
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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
    • A61K2236/50Methods 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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Abstract

The invention discloses a kind of preparation method of whortle extract, comprise the following steps:Take whortle fruit, acidic ethanol solution stirring is added to extract, stirring adds saturated sodium citrate solution after having extracted, centrifugation, discards filter residue, and concentrate adds water upper large pore resin absorption column, washed with citric acid solution, desorbed with ethanol solution, feed liquid is concentrated into no alcohol, it is whortle extract to dry.Present invention process is easy, easily operated, be easy to industrialized production, whortle extract anthocyanin (in terms of the glucoside chloride of Cyanidin 3 0) content >=36% prepared, and total anthocyanidin (in terms of Cyanidin chloride) content≤1.0%, meet American Pharmacopeia and European Pharmacopoeia requirement;Whortle extract radionuclide of the present invention137Cs contents are low, less than 10Bq/kg, meet《National food safety standard》(GB 14883.10‑2016).

Description

A kind of preparation method of whortle extract
Technical field
The present invention relates to a Plant Extracts, and in particular to a kind of preparation method of whortle extract.
Background technology
Whortle (Vaccinium myrtillus Linn.) is grown on the perennial brushwood in middle Europe One class berry.Whortle extract B ilberry Extract are that extraction is obtained using ripe whortle berry as raw material Atropurpureus powder, with eye fatigue, fatigue-relieving or leg swelling caused by prevention screen, prevents hypertension, anti-ageing to wait for a long time Function, loaded European Pharmacopoeia (EP) autonomic drug and preparation method monograph part (Monographs on Herbal Drugs and Herbal drug preparations), and it is loaded into American Pharmacopeia as dietary supplements (Dietary Supplments) (USP).Because the anthocyanin type components contained by it have the physiologically actives such as anti-oxidant, removing free radical, whortle extracts owner To be applied in functional food and medical industry.Anthocyanin content in whortle extract is made in EP and USP Regulation.Provide, detected with high performance liquid chromatography (HPLC) in EP, in terms of chloro Cyanidin -3-0- glucosides, total flower Color glycosides content is in the range of 32.4% to 39.6%.USP regulation Anthocyanin contents are not less than 36%.
Anthocyanin is the natural water colo(u)r of a class, is widely present in the organs such as root, stem, leaf, flower, the fruit of plant In cell liquid, so that it shows the colors such as red, blueness or purple.Anthocyanin is led to by pattern aglucon (aglycon) and sugar Cross the class polyphenol compound that glycosidic bond is combined into.The basic structure of natural pattern aglucon (anthocyanidin) is 3,5,7- tri- Hydroxyl-flavylium ion is muttered.The pattern being currently known have kind more than 20, but most common in plant has 6 kinds, i.e. corn flower Pigment, pelargonidin, delphinidin, paeonidin, pigment of leading a cow, malvidin.Most possibly with anthocyanidin into glycosides Monose is successively:Glucose, rhamnose, galactolipin, xylose and arabinose.1 or several can be connected on anthocyanidin molecule Glycosyl, connected mode can be monose and oligosaccharide.By changing the hydroxy number in anthocyanin molecule, the journey that methylates of hydroxyl The sugared species, quantity and the position that spend, are connected on anthocyanin molecule, the value volume and range of product for the organic acid being connected on molecule Deng substantial amounts of anthocyanin can be formed.
Anthocyanin is very unstable, and its structure is very big to itself stability influence.In general, flavylium ion is muttered sun Then stability is reduced for hydroxy number increase in ionic structure, and methylation improves and is then conducive to improving stability.Free hydroxyl The glycosylation of base will also increase the stability of anthocyanin, and the acyl group folded can be wrapped in by the sugar chain of flowing as a strap Flavylium ion is muttered the surface of skeleton, and this accumulation can prevent the eclipsed of anthocyanin caused by aquation balance conversion, to flower The color stability of color glycosides plays a protective role.It is acylated aromatic acid such as p- coumaric acids, caffeic acid, forulic acid, the mustard of anthocyanin Sub- acid, gallic acid and some aliphatic acid such as malonic acid, acetic acid, malic acid, butanedioic acid and oxalic acid also rise to the stabilization of anthocyanin Great role is arrived, the steric hindrance of acyl group makes anthocyanin be not easily susceptible to the attack of water, it is difficult to form colourless pseudobase and chalcone Structure.Other C4If the substituted stabilization for being also beneficial to anthocyanin, because can so prevent water addition, is also prevented from position Faded caused by sulfur dioxide.The stability of anthocyanin in addition to being influenceed by this body structure, also with processing and storage in Some physical and chemical factors such as pH, temperature, light, oxygen, enzyme, ascorbic acid, sugar and its catabolite, sulfur dioxide, ammonia imitate acid, phenolic acid, Metal ion, processing method etc. are relevant.
Because yellow melt salt cation lacks electronics, free anthocyanidin is very unstable.Prepared in whortle extract Cheng Zhong, should do the best and avoid the loss of the sugared aglucon of anthocyanin, so as to influence its stability.EP and USP are provided with chloro corn flower The total pattern cellulose content of element meter is less than 1% (HPLC).
Application number 200710122746.X discloses a kind of Vaccinnium vitis-idaea extract and its preparation method and application, the technology It, using red bean as raw material, is solvent with 80% ethanol water, extract solution concentrates away upper resin column after ethanol, using CHPA20 to be Ion exchange resin, uses 60% ethanol elution, removes alcohol, obtains Vaccinnium vitis-idaea extract.Containing anthocyanidin 19.6%, OPC 72.0%, anthocyanin content is not measured.
Application number 201310461582.9 discloses a kind of method that anthocyanin is extracted from whortle, including following step Suddenly:1), will with hydrochloric acid is added with refluxing extraction, ethanol solution in 40%~60% ethanol solution using whortle as raw material After extract solution concentration, by the chromatographic column filled with macroreticular resin, efflux clarification is first washed to macroreticular resin, then with 40% ~60% ethanol solution is eluted, and collects eluent, and concentration obtains crude extract after drying;2) by extractant of acetone to slightly carrying Thing is taken to carry out subcritical abstraction, extractant injection rate is 1~2 times of crude extract weight, and extraction temperature is 58~62 DEG C, extraction Pressure is 2.8~3.2MPa, and extraction time is 20~40min, and finished product is obtained after reclaiming the acetone voluntarily volatilized.The invention is passed through The processes such as ethanol solution refluxing extraction, macroporous resin adsorption, subcritical abstraction, step is simple, and the time used is short, reagent dosage Few, yield is about 0.5%, and pattern salidroside content is about 70%, and yield and purity are high, are more suitable for industrial production.But it is to anthocyanidin Do not require, and subcritical operation requires high, cost is big, complex process.
Application number 201110184914.4 discloses a kind of method that the extract containing anthocyanin is extracted from cowberry, is The existing extraction process for extracting the extract containing anthocyanin of solution generally is completed to go out in extraction process with the mode of high temperature Existing concentration step, so as to cause the problem of structure of part anthocyanin is by destruction in extraction process, the invention is provided A kind of method that the extract containing anthocyanin is extracted from cowberry, this method includes:A, cowberry is immersed in extract solution To obtain the soaking step of soak;B, with adsorption resin column layer separation soaking liquid to obtain the separating step of separating liquid;It is c, dry Dry separating liquid makes the forming step of extract formation;And separating liquid is passed through into NF membrane between b step and step c Step, the aperture of the NF membrane is 1nm or so, and above-mentioned technical problem can be effectively solved using above technical scheme.But its The NF membrane needs to be replaced and cleaned, and is not suitable for industrialization.
Application number 201410253728.5 discloses a kind of whortle extract and the method for preparing this extract.Should Invent the content of the whortle extract consistent 55%~95%, and with the finger-print of European Pharmacopoeia defined. The invention further relates to the method for preparing said extracted thing, and this method includes extracting whortle extract with macroporous absorbent resin Step, and be collected into extract solution concentration, spray drying the step of, the divinyl of big pore adsorption resin in this method The rate of charge of benzene and esters monomer is 19:1~7:3, resolving parsing agent used is the acid of ethanol or methanol or acetone The property aqueous solution.But its described macroporous absorbent resin is self-made resin, there is safety problem.
The content of the invention
The technical problems to be solved by the invention are that the technological deficiency for overcoming background technology is extracted there is provided a kind of whortle The preparation method of thing.The whortle extract anthocyanin that the present invention is prepared is (with Cyanidin 3-0- glucoside chlorinations Thing meter) content >=36%, and total anthocyanidin (in terms of Cyanidin chloride) content≤1.0%, meet American Pharmacopeia and Europe Pharmacopoeial requirements;Whortle extract radionuclide of the present invention137Cs contents are low, less than 10Bq/kg, meet《Food security state Family's standard》(GB 14883.10-2016).
The present invention solve the technological means that is used of above-mentioned technical problem for:
A kind of preparation method of whortle extract, comprises the following steps:
(1) extract for the first time:Whortle fruit is taken, acidic ethanol solution is added, stirring at normal temperature is extracted, extracts and terminates to add Enter saturated sodium citrate solution, stir, centrifugate is collected in centrifugation, and the dregs of a decoction are standby;
(2) second of extraction:First time is extracted to the filter residue after centrifugation and puts into extractor, ethanol solution is added, unlatching is stirred Mix, normal temperature is extracted, and is kept stirring for during extraction, extraction is centrifuged after terminating, and is collected filtrate, is discarded filter residue;
(3) upper prop is pre-processed:Centrifugate merging will be extracted by ethanol twice, and be concentrated into no alcohol and obtain concentrate, add water and stir Large pore resin absorption column in feed liquid, preparation, resin is cleaned before upper prop absorption with citric acid solution;
(4) upper prop is adsorbed:Large pore resin absorption column in feed liquid is adsorbed, coutroi velocity;
(5) wash:Feed liquid upper prop is eluted after terminating with citric acid solution, coutroi velocity;
(6) desorb:Elution is desorbed after finishing with ethanol solution, coutroi velocity, and observation has red liquid to be opened when occurring Begin to collect, the feed liquid that desorption is obtained is concentrated into no alcohol, it is whortle extract to dry.
In above-mentioned technical proposal, in the step (1), the saturated sodium citrate solution preparation method is:By weight The sodium citrate of 19 parts of addition in every 100 parts of water is counted, fully there is white insoluble matter as saturated lemon in the portion of seeing the bottom after dissolving Sodium solution, adds appropriate sodium citrate dissolving if all dissolvings.
In above-mentioned technical proposal, in the step (1), addition saturated sodium citrate solution regulation pH value of solution to 3.0~ 3.5。
Preferably, in the step (1), the acidic ethanol solution is that the ethanol that the concentration containing the concentrated sulfuric acid is 95% is molten Liquid.
Preferably, in the step (1), the stirring at normal temperature extraction time is 2h.
Preferably, in the step (1), it is described extract terminate to add saturated sodium citrate solution mixing time be 15~ 30min。
Preferably, in the step (2), the ethanol solution concentration is 95%.
Preferably, in the step (2), the normal temperature extraction time is 1h.
Preferably, in the step (3), the amount of water is 3 times of the volume of concentrate by volume.
Preferably, in the step (3), the pH of the citric acid solution is 3.0~3.5.
Preferably, in the step (3), the macroporous absorbent resin is nonpolar macroporous adsorption resin;More preferably Any one in HPD100, HPD300 and HPD200A;Most preferably HPD100.
Preferably, in the step (3), the weight ratio of the feed liquid and the macroporous absorbent resin is 3:1.
Preferably, in the step (4), the flow velocity is 25~35ml/min.
Preferably, in the step (5), the citric acid solution pH is 3.0~3.5.
Preferably, in the step (5), the flow velocity is 25~35ml/min.
Preferably, in the step (6), the ethanol solution concentration is 80~90%.
Preferably, in the step (6), the flow velocity is 25~35ml/min.
Its general principles:
(1) it is very unstable as the anthocyanin of active material, the physical and chemical factor in extraction process, such as temperature, pH, light, Oxygen, enzyme etc. all can produce influence to its stability.Therefore, the extraction of anthocyanin has to carry out under appropriate conditions.This hair Bright to stir extraction by adding the ethanol solution that the concentration containing the concentrated sulfuric acid is 95% at normal temperatures, stirring adds saturation after having extracted Sodium citrate solution, regulation pH value of solution prevents solution peracid from influenceing anthocyanin stability to 3.0~3.5, and the dregs of a decoction are removed in centrifugation, can To ensure active material to greatest extent --- anthocyanin effective dissolution from cell, maintain the stability of anthocyanin structure;It is dense Contracting liquid adds water upper nonpolar HPD100 large pore resin absorption columns, the citric acid solutions of pH 3.0~3.5 elution, with 80~90% Ethanol solution is parsed, and due to have selected suitable macroporous absorbent resin, eluant, eluent and strippant, flower can be improved to greatest extent The content of color glycosides, so as to obtain meeting American Pharmacopeia and the whortle extract of European Pharmacopoeia requirement;
(2) with the fast development and extensive use of nuclear technology, nuclear weapon test and nuclear accident make a large amount of artificial radioactivities Substance release enters in human environment, and radioactive pollution is produced to environment, and radionuclide can pass through the approach such as food chain and breathing Into internal.Therefore, food is not only the source of human nutrition element, is also the approach that noxious pollutant enters.The research of various countries Show, no matter ocean or continent, polluted, not only deposited in meals by artificial radionuclide from 1940s In natural radionuclide, there is also artificial radionuclide.137Cs is used as one of isotope of caesium, it is considered to be most dangerous One of nucleic.Caesium is easily absorbed by plants as the nutrition analog of potassium, into food chain, so as to be produced to human health Harm.137Cs is main fission product in high activity liquid waste, and long half time migration and is shifted, harm to the human body up to 30 years, easily Greatly, this causes people increasingly to focus on radionuclide for periodically long and harm137Cs removal.The present invention is due to have selected Suitable macroporous absorbent resin, eluant, eluent and strippant, can be reduced in whortle extract to greatest extent137Cs's contains Amount.
Compared with prior art, technical scheme has the following advantages that:
(1) present invention process is easy, easily operated, be easy to industrialized production;
(2) the whortle extract anthocyanin that the present invention is prepared is (with Cyanidin 3-0- glucoside chlorides Meter) content >=36%, and total anthocyanidin (in terms of Cyanidin chloride) content≤1.0%, meet American Pharmacopeia and European medicine Allusion quotation requirement;
(3) whortle extract radionuclide of the present invention137Cs contents are low, less than 10Bq/kg, meet《Food security National standard》(GB 14883.10-2016).
Embodiment
Content for a better understanding of the present invention, is described further with reference to specific embodiment.It should be understood that these Embodiment is only used for that the present invention is further described, rather than limitation the scope of the present invention.In addition, it is to be understood that reading this After the content of invention, person skilled in art makes some nonessential changes or adjustment to the present invention, still falls within the present invention Protection domain.
Embodiment 1
(1) extract for the first time:800g whortle fruits are taken, the stirring of the ethanol solutions of 2.4L 95% is added, adds 6.5g The concentrated sulfuric acid, stirring at normal temperature extracts 2h, extracts and terminates to add saturated sodium citrate solution 25g, regulation pH value of solution is stirred to 3.0~3.5 15min is mixed, is centrifuged, centrifugate is collected, filter residue is standby;
(2) second of extraction:First time is extracted to the filter residue after centrifugation and puts into extractor, the ethanol of 3.6L 95% is added molten Liquid, opens stirring, and normal temperature extracts 1h, is kept stirring for during extraction, and extraction is centrifuged after terminating, and is collected filtrate, is discarded filter residue;
(3) upper prop is pre-processed:Centrifugate merging will be extracted by ethanol twice, and be concentrated into no alcohol and obtain concentrate, add concentrate The water that 3 times of volume stirs to obtain large pore resin absorption column in feed liquid, preparation, and the citric acid solutions of pH 3.0~3.5 are used before upper prop absorption Clean resin;
(4) upper prop is adsorbed:HPD100 posts in feed liquid are adsorbed, coutroi velocity is 25~30ml/min;
(5) wash:Feed liquid upper prop is eluted after terminating with 1.5L pH 3.0~3.5 citric acid solution, coutroi velocity For 25~30ml/min;
(6) desorb:Elution is desorbed after finishing with the ethanol solutions of 3.6L 80%, and coutroi velocity is 25~30ml/min, Observation has red liquid to start collection when occurring, and the feed liquid that desorption is obtained is concentrated into no alcohol, and it is that whortle is extracted to dry Thing.
The anthocyanin that the present embodiment is prepared (counts) content as 37.1% using Cyanidin 3-0- glucoside chlorides, Total anthocyanidin (in terms of Cyanidin chloride) content 0.6%, radionuclide137Cs contents are 8.9Bq/kg.
Embodiment 2
(1) extract for the first time:1000g whortle fruits are taken, the stirring of the ethanol solutions of 3L 95% is added, adds 7.5g The concentrated sulfuric acid, stirring at normal temperature extracts 2h, extracts and terminates to add saturated sodium citrate solution 30g, regulation pH value of solution is stirred to 3.0~3.5 30min is mixed, is centrifuged, centrifugate is collected, filter residue is standby;
(2) second of extraction:First time is extracted to the filter residue after centrifugation and puts into extractor, the ethanol of 4.5L 95% is added molten Liquid, opens stirring, and normal temperature extracts 1h, is kept stirring for during extraction, and extraction is centrifuged after terminating, and is collected filtrate, is discarded filter residue;
(3) upper prop is pre-processed:Centrifugate merging will be extracted by ethanol twice, and be concentrated into no alcohol and obtain concentrate, add concentrate The water that 3 times of volume stirs to obtain large pore resin absorption column in feed liquid, preparation, and the citric acid solutions of pH 3.0~3.5 are used before upper prop absorption Clean resin;
(4) upper prop is adsorbed:HPD300 posts in feed liquid are adsorbed, coutroi velocity is 30~35ml/min;
(5) wash:Feed liquid upper prop is eluted after terminating with 1.8L pH 3.0~3.5 citric acid solution, coutroi velocity For 30~35ml/min;
(6) desorb:Elution is desorbed after finishing with the ethanol solutions of 4.1L 90%, and coutroi velocity is 30~35ml/min, Observation has red liquid to start collection when occurring, and the feed liquid that desorption is obtained is concentrated into no alcohol, and it is that whortle is extracted to dry Thing.
The anthocyanin that the present embodiment is prepared (counts) content as 37.5% using Cyanidin 3-0- glucoside chlorides, Total anthocyanidin (in terms of Cyanidin chloride) content 0.7%, radionuclide137Cs contents are 9.3Bq/kg.
Embodiment 3
(1) extract for the first time:900g whortle fruits are taken, the stirring of the ethanol solutions of 2.8L 95% is added, adds 7.0g The concentrated sulfuric acid, stirring at normal temperature extracts 2h, extracts and terminates to add saturated sodium citrate solution 27g, adjusts pH value of solution to 3.0~3.5, 18min is stirred, centrifugate is collected in centrifugation, and filter residue is standby;
(2) second of extraction:First time is extracted to the filter residue after centrifugation and puts into extractor, the ethanol of 3.8L 95% is added molten Liquid, opens stirring, and normal temperature extracts 1h, is kept stirring for during extraction, and extraction is centrifuged after terminating, and is collected filtrate, is discarded filter residue;
(3) upper prop is pre-processed:Centrifugate merging will be extracted by ethanol twice, and be concentrated into no alcohol and obtain concentrate, add concentrate The water that 3 times of volume stirs to obtain large pore resin absorption column in feed liquid, preparation, and the citric acid solutions of pH 3.0~3.5 are used before upper prop absorption Clean resin;
(4) upper prop is adsorbed:HPD200A posts in feed liquid are adsorbed, coutroi velocity is 28~33ml/min;
(5) wash:Feed liquid upper prop is eluted after terminating with 2.0L pH 3.0~3.5 citric acid solution, coutroi velocity For 28~33ml/min;
(6) desorb:Elution is desorbed after finishing with the ethanol solutions of 4.5L 85%, and coutroi velocity is 28~33ml/min, Observation has red liquid to start collection when occurring, and the feed liquid that desorption is obtained is concentrated into no alcohol, and it is that whortle is extracted to dry Thing.
The anthocyanin that the present embodiment is prepared (counts) content as 37.2% using Cyanidin 3-0- glucoside chlorides, Total anthocyanidin (in terms of Cyanidin chloride) content 0.8%, radionuclide137Cs contents are 8.5Bq/kg.
HPD100, HPD300 and HPD200A described in embodiment 1~3 are purchased from the limited public affairs of the precious grace sorbing material science and technology in Cangzhou Department.
Saturated sodium citrate solution preparation method is described in embodiment 1~3:9.5g citric acid is added in water per 50g Sodium, fully dissolving after the portion of seeing the bottom have white insoluble matter as saturated sodium citrate solution, such as all dissolve then add it is appropriate Sodium citrate dissolves.
The limitation of described above not to invention, the present invention is also not limited to the example above.The common skill of the art Art personnel are in the essential scope of invention, and the variations, modifications, additions or substitutions made should also belong to protection scope of the present invention.

Claims (10)

1. a kind of preparation method of whortle extract, it is characterised in that comprise the following steps:
(1) extract for the first time:Whortle fruit is taken, acidic ethanol solution is added, stirring at normal temperature is extracted, end addition is extracted full And sodium citrate solution, stir, centrifugate is collected in centrifugation, and filter residue is standby;
(2) second of extraction:First time is extracted to the filter residue after centrifugation and puts into extractor, ethanol solution is added, opens stirring, often Temperature is extracted, and is kept stirring for during extraction, and extraction is centrifuged after terminating, and is collected filtrate, is discarded filter residue;
(3) upper prop is pre-processed:Centrifugate merging will be extracted by ethanol twice, and be concentrated into no alcohol and obtain concentrate, add water and stir to obtain feed liquid, Large pore resin absorption column in preparation, resin is cleaned before upper prop absorption with citric acid solution;
(4) upper prop is adsorbed:Large pore resin absorption column in feed liquid is adsorbed, coutroi velocity;
(5) wash:Feed liquid upper prop is eluted after terminating with citric acid solution, coutroi velocity;
(6) desorb:Elution is desorbed after finishing with ethanol solution, coutroi velocity, and observation has red liquid to start receipts when occurring Collection, the feed liquid that desorption is obtained is concentrated into no alcohol, and it is whortle extract to dry.
2. a kind of preparation method of whortle extract as claimed in claim 1, it is characterised in that in the step (1), The acidic ethanol solution is the ethanol solution that the concentration containing the concentrated sulfuric acid is 95%.
3. a kind of preparation method of whortle extract as claimed in claim 1, it is characterised in that in the step (3), The pH of the citric acid solution is 3.0~3.5.
4. a kind of preparation method of whortle extract as claimed in claim 1, it is characterised in that in the step (3), The macroporous absorbent resin is nonpolar macroporous adsorption resin.
5. a kind of preparation method of whortle extract as claimed in claim 1, it is characterised in that in the step (3), The weight ratio of the feed liquid and the macroporous absorbent resin is 3:1.
6. a kind of preparation method of whortle extract as claimed in claim 1, it is characterised in that in the step (4), The flow velocity is 25~35ml/min.
7. a kind of preparation method of whortle extract as claimed in claim 1, it is characterised in that in the step (5), The citric acid solution pH is 3.0~3.5.
8. a kind of preparation method of whortle extract as claimed in claim 1, it is characterised in that in the step (5), The flow velocity is 25~35ml/min.
9. a kind of preparation method of whortle extract as claimed in claim 1, it is characterised in that in the step (6), The ethanol solution concentration is 80~90%.
10. a kind of preparation method of whortle extract as claimed in claim 1, it is characterised in that the step (6) In, the flow velocity is 25~35ml/min.
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CN108174896A (en) * 2018-02-06 2018-06-19 浦江县泰如食品科技有限公司 A kind of ship biscuit preparation method full of nutrition
CN110372659A (en) * 2019-08-07 2019-10-25 太仓新亚逊生物科技有限公司 The extraction process of blueberry anthocyanin
CN110498826A (en) * 2018-09-12 2019-11-26 陕西源邦生物技术有限公司 A kind of preparation method of whortle anthocyanin and its processing method of by-product
RU2744613C1 (en) * 2020-07-10 2021-03-11 Федеральное государственное бюджетное научное учреждение "Томский национальный исследовательский медицинский центр Российской академии наук" (Томский НИМЦ) Phyto remedy with cerebroprotective action
CN113350227A (en) * 2021-06-07 2021-09-07 上海其然生物科技有限公司 Cleansing oil containing oil-soluble and water-soluble vaccinium myrtillus active ingredients and preparation method thereof
CN113786371A (en) * 2021-07-05 2021-12-14 中国科学院烟台海岸带研究所 Composition for preparing blueberry seaweed mask, mask and preparation method
CN114031952A (en) * 2022-01-10 2022-02-11 罗麦(北京)营养食品研究有限公司 Method for extracting anthocyanin from plant

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CN101215424A (en) * 2008-01-16 2008-07-09 华东师范大学 Method for extracting and refining bilberry schlempe anthocyanidin
CN105287690A (en) * 2014-06-06 2016-02-03 天津南开允公医药科技有限公司 Bilberry extract and preparation method thereof

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CN1294131A (en) * 1999-10-20 2001-05-09 中国科学院沈阳应用生态研究所 Process for extracting anthoxyanin from cowbeery
EP1328282A1 (en) * 2000-08-31 2003-07-23 Hauser, Inc. Efficient method for producing compositions enriched in anthocyanins
CN1517343A (en) * 2003-01-13 2004-08-04 大兴安岭华野生物工程有限公司 Extraction method of huckleberry anthocyanidin
CN101215424A (en) * 2008-01-16 2008-07-09 华东师范大学 Method for extracting and refining bilberry schlempe anthocyanidin
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Publication number Priority date Publication date Assignee Title
CN108174896A (en) * 2018-02-06 2018-06-19 浦江县泰如食品科技有限公司 A kind of ship biscuit preparation method full of nutrition
CN110498826A (en) * 2018-09-12 2019-11-26 陕西源邦生物技术有限公司 A kind of preparation method of whortle anthocyanin and its processing method of by-product
CN110498826B (en) * 2018-09-12 2023-01-03 陕西源邦生物技术有限公司 Preparation method of vaccinium myrtillus anthocyanin and treatment method of byproducts of vaccinium myrtillus anthocyanin
CN110372659A (en) * 2019-08-07 2019-10-25 太仓新亚逊生物科技有限公司 The extraction process of blueberry anthocyanin
RU2744613C1 (en) * 2020-07-10 2021-03-11 Федеральное государственное бюджетное научное учреждение "Томский национальный исследовательский медицинский центр Российской академии наук" (Томский НИМЦ) Phyto remedy with cerebroprotective action
CN113350227A (en) * 2021-06-07 2021-09-07 上海其然生物科技有限公司 Cleansing oil containing oil-soluble and water-soluble vaccinium myrtillus active ingredients and preparation method thereof
CN113786371A (en) * 2021-07-05 2021-12-14 中国科学院烟台海岸带研究所 Composition for preparing blueberry seaweed mask, mask and preparation method
CN114031952A (en) * 2022-01-10 2022-02-11 罗麦(北京)营养食品研究有限公司 Method for extracting anthocyanin from plant

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