CN105708795A - Pure natural blueberry anthocyanin aglycone oral solution and preparation method - Google Patents
Pure natural blueberry anthocyanin aglycone oral solution and preparation method Download PDFInfo
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- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
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- A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline
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- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/45—Ericaceae or Vacciniaceae (Heath or Blueberry family), e.g. blueberry, cranberry or bilberry
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- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/26—Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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Abstract
The invention discloses a pure natural blueberry anthocyanin aglycone oral solution and a preparation method. The blueberry anthocyanin aglycone oral solution is prepared from, by weight, 80-85 parts of concentrated blueberry anthocyanin aglycone hydrolysate, 500-1000 parts of honey, 350-500 parts of white granulated sugar and 100-200 parts of purified water. The preparation method comprises the steps of 1 pretreatment, 2 purification, 3 hydrolysis and 4 preparation of the oral solution. The pure natural blueberry anthocyanin aglycone oral solution has the advantages that a solvent extraction and chromatography combined technique is adopted to prepare the pure natural anthocyanin aglycone oral solution easy to absorb on the basis that an operation process is simplified and the cost is saved, and the oral solution has a higher nutritional value and a health-care function and is suitable for wide-range populations.
Description
Technical field
The present invention relates to a kind of anthocyanin primordial oral liquid and preparation method, particularly to the indigo plant of a kind of pure natural
Certain kind of berries anthocyanin primordial oral liquid and preparation method.
Background technology
Along with people's living standard improves constantly, people are the strongest to the pursuit of natural organic substance.Closely
Nian Lai, the organic substance of the natural botanical source useful to human body, increasingly favored by people.
At present, the researchers of various countries' anthocyanidin are just getting down to from plant, especially extract flower from blue berry
Blue or green element component, makes various eye care product, for the treatment of various ophthalmic diseasess.There are some researches show, flower
Blue or green element can promote the absorption of injection Vitamin B_6, strengthens the resistivity of blood vessel, lowers the fragility of blood capillary,
Maintain the saturating property of energy of blood vessel, reduce the incidence rate of cardiovascular disease, moreover it is possible to improve varicosis or edema, fall
The sickness rate of low diabetes etc. act on.The annual production of China's wild blueberry has reached 20,000 tons, and in increasing year by year
Add trend.In wild blueberry fruit, anthocyanidin content is the abundantest, and biological activity is high.Existing anthocyanidin
Separating and purifying technology mainly for anthocyanidin glucosides class material, obtained anthocyanidin product commonly exists pure
Spend the problems such as low, poor activity, the highest in the using value of foods and cosmetics industry.Anthocyanidin glucosides is
The glucosides that in plant, anthocyanidin cation is combined into by glycosidic bond with monosaccharide, low in human body internal absorption factor,
Bioavailability is the highest, after only forming anthocyanidin aglycon by intestinal degraded desaccharide, is just prone to by human body
Absorb, utilize.Anthocyanidin aglycon free in natural plants seldom exists.And the anthocyanin of synthetic
Unit, toxic and side effects is relatively big, can not service for people, and be forbidden by World Health Organization (WHO).Therefore, system
The vaccinium oxycoccus pigment aglycon product of standby pure natural is extremely urgent.
Recently, the product about vaccinium oxycoccus pigment glucosides is increasing on the market, and many based on oral liquid.
Oral liquid has that taking dose is little, it is very fast to absorb, steady quality, preservation easy to carry and use, easy, suitable
Close the advantages such as industrialized production, it has also become preparation develops one of dosage form faster.And it is easy about activity height
The vaccinium oxycoccus pigment aglycon oral liquid absorbed is few.Therefore, exploitation pure natural vaccinium oxycoccus pigment aglycon oral liquid
There is important market using value.
The existing patent about anthocyanidin glucosides oral liquid is mainly by following several: patent 1 (application number:
201010179439.7 date of publication: 2010.09.22) entitled: blueberry anthocyanin oral solution, patent 2
(application number: 200910225886.9, date of publication: 2010.11.03) entitled: a kind of anthocyanidin mouth
Take liquid and beverage and production method thereof, patent 3 (application number: 201510339437.2, date of publication:
2015.09.09) entitled: a kind of anthocyanidin oral liquid good for eyes and preparation method thereof, three inventions are all
With vaccinium oxycoccus pigment glucosides for primary healthcare composition, biological activity is relatively low, and absorption of human body utilization rate is the most relatively
Low.Patent about anthocyanidin aglycon mainly has following: patent 1 (application number: 200910185829.2,
Date of publication: 2010.06.30) entitled: the microorganism of Anthocyanin, or/and biological enzyme extracting method, is
The industrialization extractive technique of the i.e. active aglycone of anthocyanidin, patent 2 (application number: 201210516999.6, announce
Day: 2014.06.04) entitled: the extracting method of a kind of cation anthocyanidin aglycon, patent 3 (application number:
201310112792.7, date of publication: 2014.09.24) entitled: the extraction of natural anthocyanidin active aglycone
Method, three above patent is the technology of preparing of active aglycone, belongs to technical field of bioengineering, three
The general character of patent is, needs to use microorganism, enzyme preparation, antibacterial etc. in production process, its production procedure complexity,
Cycle length, production cost are higher, production efficiency is relatively low, it is also possible to have microorganism and air ambient is caused two
Secondary pollution, enzyme and the bacteriological filter potential problems such as not exclusively, are detrimental to health.
Summary of the invention
The invention aims to solve existing anthocyanin primordial oral liquid and exist many in preparation process
Problem and the vaccinium oxycoccus pigment aglycon oral liquid of a kind of pure natural that provides and preparation method.
The vaccinium oxycoccus pigment aglycon oral liquid of the pure natural that the present invention provides includes concentration vaccinium oxycoccus pigment aglycon
Hydrolyzed solution, Mel, white sugar and pure water, the most various raw materials proportioning by weight is: concentrate blue berry
Anthocyanidin aglycon hydrolyzed solution 80-85 part；Mel 500-1000 part；White sugar 350-500 part；Pure water
100-200 part.
Concentrating vaccinium oxycoccus pigment aglycon weight content in vaccinium oxycoccus pigment aglycon hydrolyzed solution is 5%-8%.
The preparation method of the vaccinium oxycoccus pigment aglycon oral liquid of the pure natural that the present invention provides, its preparation method is such as
Under:
Step one, pretreatment: select fresh or freezing Blueberry, remove decayed fruit, and impurity, clean,
Grinding is smashed to pieces, in pulp shape；
Step 2, purification: in pulp, first add acidic ethanol solution, to dissolve the anthocyanidin in raw material；
In acidic ethanol solution, pulp and acidic ethanol solution volume ratio are 1:10-1:15, extract 3-5 under normal temperature condition
Secondary, the time is 2-4h/ time；It is evaporated to 1/15-1/10, room temperature equal-volume ethyl acetate extraction 3-5
Secondary, the time is 6-12h/ time；Carry out macroporous resin column and gel chromatography column chromatography, each loading the most successively
Amount is less than the 10%-20% of post content volume, successively with acidifying distilled water, 20%-40% ethanol elution, stream
Speed is 0.5-1BV/h；
Step 3, hydrolysis: anthocyanidin solution decompression after purification in step 2 is concentrated into original volume
5%-10%, is subsequently adding ethanol solution and citric acid solution, and in ethanol solution, ethanol with the volume ratio of water is
1:1-1:3/7, ethanol solution is 1:3-1:5 with the volume ratio of citric acid solution, and citric acid solution concentration is
4.5-5.5mol/L, after previous solu mix homogeneously fully reacts 1-3h in being placed on the water-bath of 80-100 DEG C,
Take out cooling rapidly；
Step 4, the preparation of oral liquid: mistake in gained hydrolyzed solution in employing decrease temperature crystalline method removing step three
The citric acid of amount, and then concentrating under reduced pressure hydrolyzed solution is 5%-8% to vaccinium oxycoccus pigment aglycon weight content；Reduce pressure dense
Contracting temperature is 50 DEG C, vacuum is-0.09MPa, and each raw material according to weight is, concentrates blue berry cyanine
Element aglycon hydrolyzed solution 80-85 part；Add Mel 500-1000 part；White sugar 350-500 part；Pure water
100-200 part；Mixing raw material, UHT sterilizing, sterile filling enter bottle obtain pure natural vaccinium oxycoccus pigment aglycon be administered orally
Liquid.
In step 2 big pore resin entitled Amberlite XAD-7HP ion exchange macroporous resin or
AB-8 macroporous resin, gel chromatography filler used is Sephadex LH-20；Souring soln used is
0.4%-0.8%wt acidified with citric acid solution.
Beneficial effects of the present invention:
Present invention employs solvent extraction and chromatography multiple techniques, simplify operating procedure and cost-effective base
On plinth, prepare pure natural, the anthocyanin primordial oral liquid easily absorbed, there is better nutritivity and be worth and health care
Function, is suitable for crowd extensive.
Accompanying drawing explanation
Fig. 1 is the pure natural vaccinium oxycoccus pigment aglycon oral liquid high-efficient liquid phase chromatogram that the present invention prepares.
The anthocyanidin aglycon monomer that in figure, sequence number 1-5 is the most corresponding is as follows:
1. delphinidin, 2. cyanidin, 3. lead a cow florigen, 4. paeonidin, 5. enidin.
Detailed description of the invention
Embodiment one:
The vaccinium oxycoccus pigment aglycon oral liquid of the pure natural that the present invention provides includes concentration vaccinium oxycoccus pigment aglycon
Hydrolyzed solution, Mel, white sugar and pure water, the most various raw materials proportioning by weight is: concentrate blue berry
Anthocyanidin aglycon hydrolyzed solution 80 parts；Mel 500 parts；White sugar 350 parts；Pure water 100 parts.
Concentrating vaccinium oxycoccus pigment aglycon weight content in vaccinium oxycoccus pigment aglycon hydrolyzed solution is 5%.
The preparation method of the vaccinium oxycoccus pigment aglycon oral liquid of the pure natural that the present invention provides, its preparation method is such as
Under:
Step one, pretreatment: select fresh or freezing Blueberry, remove decayed fruit, and impurity, clean,
Grinding is smashed to pieces, in pulp shape；
Step 2, purification: in pulp, first add acidic ethanol solution, to dissolve the anthocyanidin in raw material；
In acidic ethanol solution, pulp and acidic ethanol solution volume ratio are 1:10-1:15, extract 3-5 under normal temperature condition
Secondary, the time is 2-4h/ time；It is evaporated to 1/15-1/10, room temperature equal-volume ethyl acetate extraction 3-5
Secondary, the time is 6-12h/ time；Carry out macroporous resin column and gel chromatography column chromatography, each loading the most successively
Amount is less than the 10%-20% of post content volume, successively with acidifying distilled water, 20%-40% ethanol elution, stream
Speed is 0.5-1BV/h；
Step 3, hydrolysis: anthocyanidin solution decompression after purification in step 2 is concentrated into original volume
5%-10%, is subsequently adding ethanol solution and citric acid solution, and in ethanol solution, ethanol with the volume ratio of water is
1:1-1:3/7, ethanol solution is 1:3-1:5 with the volume ratio of citric acid solution, and citric acid solution concentration is
4.5-5.5mol/L, after previous solu mix homogeneously fully reacts 1-3h in being placed on the water-bath of 80-100 DEG C,
Take out cooling rapidly；
Step 4, the preparation of oral liquid: mistake in gained hydrolyzed solution in employing decrease temperature crystalline method removing step three
The citric acid of amount, and then concentrating under reduced pressure hydrolyzed solution is 5% to vaccinium oxycoccus pigment aglycon weight content；Concentrating under reduced pressure
Temperature is 50 DEG C, vacuum is-0.09MPa, and each raw material according to weight is, concentrates vaccinium oxycoccus pigment
Aglycon hydrolyzed solution 80 parts；Add Mel 500 parts；White sugar 350 parts；Pure water 100 parts；Mix former
Material, UHT sterilizing, sterile filling enters bottle and obtains pure natural vaccinium oxycoccus pigment aglycon oral liquid.
In step 2 big pore resin entitled Amberlite XAD-7HP ion exchange macroporous resin or
AB-8 macroporous resin, gel chromatography filler used is Sephadex LH-20；Souring soln used is
0.4%-0.8%wt acidified with citric acid solution.
Embodiment two:
The vaccinium oxycoccus pigment aglycon oral liquid of the pure natural that the present invention provides includes concentration vaccinium oxycoccus pigment aglycon
Hydrolyzed solution, Mel, white sugar and pure water, the most various raw materials proportioning by weight is: concentrate blue berry
Anthocyanidin aglycon hydrolyzed solution 85 parts；Mel 1000 parts；White sugar 500 parts；Pure water 200 parts.
Concentrating vaccinium oxycoccus pigment aglycon weight content in vaccinium oxycoccus pigment aglycon hydrolyzed solution is 8%.
The preparation method of the vaccinium oxycoccus pigment aglycon oral liquid of the pure natural that the present invention provides, its preparation method is such as
Under:
Step one, pretreatment: select fresh or freezing Blueberry, remove decayed fruit, and impurity, clean,
Grinding is smashed to pieces, in pulp shape；
Step 2, purification: in pulp, first add acidic ethanol solution, to dissolve the anthocyanidin in raw material；
In acidic ethanol solution, pulp and acidic ethanol solution volume ratio are 1:10-1:15, extract 3-5 under normal temperature condition
Secondary, the time is 2-4h/ time；It is evaporated to 1/15-1/10, room temperature equal-volume ethyl acetate extraction 3-5
Secondary, the time is 6-12h/ time；Carry out macroporous resin column and gel chromatography column chromatography, each loading the most successively
Amount is less than the 10%-20% of post content volume, successively with acidifying distilled water, 20%-40% ethanol elution, stream
Speed is 0.5-1BV/h；
Step 3, hydrolysis: anthocyanidin solution decompression after purification in step 2 is concentrated into original volume
5%-10%, is subsequently adding ethanol solution and citric acid solution, and in ethanol solution, ethanol with the volume ratio of water is
1:1-1:3/7, ethanol solution is 1:3-1:5 with the volume ratio of citric acid solution, and citric acid solution concentration is
4.5-5.5mol/L, after previous solu mix homogeneously fully reacts 1-3h in being placed on the water-bath of 80-100 DEG C,
Take out cooling rapidly；
Step 4, the preparation of oral liquid: mistake in gained hydrolyzed solution in employing decrease temperature crystalline method removing step three
The citric acid of amount, and then concentrating under reduced pressure hydrolyzed solution is 8% to vaccinium oxycoccus pigment aglycon weight content；Concentrating under reduced pressure
Temperature is 50 DEG C, vacuum is-0.09MPa, and each raw material according to weight is, concentrates vaccinium oxycoccus pigment
Aglycon hydrolyzed solution 85 parts；Add Mel 1000 parts；White sugar 500 parts；Pure water 200 parts；Mix former
Material, UHT sterilizing, sterile filling enters bottle and obtains pure natural vaccinium oxycoccus pigment aglycon oral liquid.
In step 2 big pore resin entitled Amberlite XAD-7HP ion exchange macroporous resin or
AB-8 macroporous resin, gel chromatography filler used is Sephadex LH-20；Souring soln used is
0.4%-0.8%wt acidified with citric acid solution.
Embodiment three:
The vaccinium oxycoccus pigment aglycon oral liquid of the pure natural that the present invention provides includes concentration vaccinium oxycoccus pigment aglycon
Hydrolyzed solution, Mel, white sugar and pure water, the most various raw materials proportioning by weight is: concentrate blue berry
Anthocyanidin aglycon hydrolyzed solution 83 parts；Mel 750 parts；White sugar 430 parts；Pure water 150 parts.
Concentrating vaccinium oxycoccus pigment aglycon weight content in vaccinium oxycoccus pigment aglycon hydrolyzed solution is 6%.
The preparation method of the vaccinium oxycoccus pigment aglycon oral liquid of the pure natural that the present invention provides, its preparation method is such as
Under:
Step one, pretreatment: select fresh or freezing Blueberry, remove decayed fruit, and impurity, clean,
Grinding is smashed to pieces, in pulp shape；
Step 2, purification: in pulp, first add acidic ethanol solution, to dissolve the anthocyanidin in raw material；
In acidic ethanol solution, pulp and acidic ethanol solution volume ratio are 1:10-1:15, extract 3-5 under normal temperature condition
Secondary, the time is 2-4h/ time；It is evaporated to 1/15-1/10, room temperature equal-volume ethyl acetate extraction 3-5
Secondary, the time is 6-12h/ time；Carry out macroporous resin column and gel chromatography column chromatography, each loading the most successively
Amount is less than the 10%-20% of post content volume, successively with acidifying distilled water, 20%-40% ethanol elution, stream
Speed is 0.5-1BV/h；
Step 3, hydrolysis: anthocyanidin solution decompression after purification in step 2 is concentrated into original volume
5%-10%, is subsequently adding ethanol solution and citric acid solution, and in ethanol solution, ethanol with the volume ratio of water is
1:1-1:3/7, ethanol solution is 1:3-1:5 with the volume ratio of citric acid solution, and citric acid solution concentration is
4.5-5.5mol/L, after previous solu mix homogeneously fully reacts 1-3h in being placed on the water-bath of 80-100 DEG C,
Take out cooling rapidly；
Step 4, the preparation of oral liquid: mistake in gained hydrolyzed solution in employing decrease temperature crystalline method removing step three
The citric acid of amount, and then concentrating under reduced pressure hydrolyzed solution is 6% to vaccinium oxycoccus pigment aglycon weight content；Concentrating under reduced pressure
Temperature is 50 DEG C, vacuum is-0.09MPa, and each raw material according to weight is, concentrates vaccinium oxycoccus pigment
Aglycon hydrolyzed solution 83 parts；Add Mel 750 parts；White sugar 430 parts；Pure water 150 parts；Mix former
Material, UHT sterilizing, sterile filling enters bottle and obtains pure natural vaccinium oxycoccus pigment aglycon oral liquid.
In step 2 big pore resin entitled Amberlite XAD-7HP ion exchange macroporous resin or
AB-8 macroporous resin, gel chromatography filler used is Sephadex LH-20；Souring soln used is
0.4%-0.8%wt acidified with citric acid solution.
Claims (4)
1. the vaccinium oxycoccus pigment aglycon oral liquid of a pure natural, it is characterised in that: include concentration blue berry flower
Blue or green element aglycon hydrolyzed solution, Mel, white sugar and pure water, the most various raw materials proportioning by weight is:
Concentrate vaccinium oxycoccus pigment aglycon hydrolyzed solution 80-85 part；Mel 500-1000 part；White sugar 350-500 part；
Pure water 100-200 part.
The vaccinium oxycoccus pigment aglycon oral liquid of a kind of pure natural the most according to claim 1, its feature exists
In: in described concentration vaccinium oxycoccus pigment aglycon hydrolyzed solution, vaccinium oxycoccus pigment aglycon weight content is 5%-8%.
3. the preparation method of the vaccinium oxycoccus pigment aglycon oral liquid of a pure natural, it is characterised in that: it is prepared
Method is as follows:
Step one, pretreatment: select fresh or freezing Blueberry, remove decayed fruit, and impurity, clean,
Grinding is smashed to pieces, in pulp shape；
Step 2, purification: in pulp, first add acidic ethanol solution, to dissolve the anthocyanidin in raw material；
In acidic ethanol solution, pulp and acidic ethanol solution volume ratio are 1:10-1:15, extract 3-5 under normal temperature condition
Secondary, the time is 2-4h/ time；It is evaporated to 1/15-1/10, room temperature equal-volume ethyl acetate extraction 3-5
Secondary, the time is 6-12h/ time；Carry out macroporous resin column and gel chromatography column chromatography, each loading the most successively
Amount is less than the 10%-20% of post content volume, successively with acidifying distilled water, 20%-40% ethanol elution, stream
Speed is 0.5-1BV/h；
Step 3, hydrolysis: anthocyanidin solution decompression after purification in step 2 is concentrated into original volume
5%-10%, is subsequently adding ethanol solution and citric acid solution, and in ethanol solution, ethanol with the volume ratio of water is
1:1-1:3/7, ethanol solution is 1:3-1:5 with the volume ratio of citric acid solution, and citric acid solution concentration is
4.5-5.5mol/L, after previous solu mix homogeneously fully reacts 1-3h in being placed on the water-bath of 80-100 DEG C,
Take out cooling rapidly；
Step 4, the preparation of oral liquid: mistake in gained hydrolyzed solution in employing decrease temperature crystalline method removing step three
The citric acid of amount, and then concentrating under reduced pressure hydrolyzed solution is 5%-8% to vaccinium oxycoccus pigment aglycon weight content；Reduce pressure dense
Contracting temperature is 50 DEG C, vacuum is-0.09MPa, and each raw material according to weight is, concentrates blue berry cyanine
Element aglycon hydrolyzed solution 80-85 part；Add Mel 500-1000 part；White sugar 350-500 part；Pure water
100-200 part；Mixing raw material, UHT sterilizing, sterile filling enter bottle obtain pure natural vaccinium oxycoccus pigment aglycon be administered orally
Liquid.
The vaccinium oxycoccus pigment aglycon oral liquor of a kind of pure natural the most according to claim 3,
It is characterized in that: in described step 2, big pore resin entitled Amberlite XAD-7HP ion is handed over
Changing macroporous resin or AB-8 macroporous resin, gel chromatography filler used is Sephadex LH-20；Acid used
Changing solution is 0.4%-0.8%wt acidified with citric acid solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610160610.7A CN105708795A (en) | 2016-03-21 | 2016-03-21 | Pure natural blueberry anthocyanin aglycone oral solution and preparation method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610160610.7A CN105708795A (en) | 2016-03-21 | 2016-03-21 | Pure natural blueberry anthocyanin aglycone oral solution and preparation method |
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| CN105708795A true CN105708795A (en) | 2016-06-29 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111053248A (en) * | 2018-10-16 | 2020-04-24 | 东莞市维康医疗投资有限公司 | Earthworm protein oral liquid and preparation method thereof |
| CN109965285A (en) * | 2019-04-12 | 2019-07-05 | 广东农工商职业技术学院 | A kind of natural anti-oxidation black potato anthocyanin oral solution and preparation method thereof |
| CN111387316A (en) * | 2020-04-29 | 2020-07-10 | 穆延东 | Formula of honey product containing anthocyanin |
| CN112314909A (en) * | 2020-11-02 | 2021-02-05 | 穆延东 | A beverage containing anthocyanin-containing Mel |
| CN114028446A (en) * | 2021-11-19 | 2022-02-11 | 四川省农业科学院经济作物育种栽培研究所 | Blueberry oral liquid and preparation method thereof |
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