CN115466240A - Method for extracting anthocyanin from blueberries - Google Patents
Method for extracting anthocyanin from blueberries Download PDFInfo
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- CN115466240A CN115466240A CN202211287651.4A CN202211287651A CN115466240A CN 115466240 A CN115466240 A CN 115466240A CN 202211287651 A CN202211287651 A CN 202211287651A CN 115466240 A CN115466240 A CN 115466240A
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- 235000010208 anthocyanin Nutrition 0.000 title claims abstract description 52
- 229930002877 anthocyanin Natural products 0.000 title claims abstract description 52
- 239000004410 anthocyanin Substances 0.000 title claims abstract description 52
- 150000004636 anthocyanins Chemical class 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 33
- 235000003095 Vaccinium corymbosum Nutrition 0.000 title claims abstract description 31
- 235000017537 Vaccinium myrtillus Nutrition 0.000 title claims abstract description 31
- 235000021014 blueberries Nutrition 0.000 title claims abstract description 31
- 240000000851 Vaccinium corymbosum Species 0.000 title claims abstract description 30
- 239000000243 solution Substances 0.000 claims abstract description 54
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 51
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 34
- DZGCGKFAPXFTNM-UHFFFAOYSA-N ethanol;hydron;chloride Chemical compound Cl.CCO DZGCGKFAPXFTNM-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000284 extract Substances 0.000 claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- 238000002386 leaching Methods 0.000 claims abstract description 15
- 239000000287 crude extract Substances 0.000 claims abstract description 14
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 239000002537 cosmetic Substances 0.000 claims abstract description 5
- 230000006837 decompression Effects 0.000 claims abstract description 5
- 239000003814 drug Substances 0.000 claims abstract description 5
- 238000007865 diluting Methods 0.000 claims abstract description 4
- 238000005360 mashing Methods 0.000 claims abstract 2
- 238000002360 preparation method Methods 0.000 claims description 4
- 229930014669 anthocyanidin Natural products 0.000 claims description 3
- 150000001453 anthocyanidins Chemical class 0.000 claims description 3
- 235000008758 anthocyanidins Nutrition 0.000 claims description 3
- 230000003078 antioxidant effect Effects 0.000 claims description 3
- 230000004438 eyesight Effects 0.000 claims description 3
- 230000001093 anti-cancer Effects 0.000 claims description 2
- 239000003963 antioxidant agent Substances 0.000 claims 1
- 235000006708 antioxidants Nutrition 0.000 claims 1
- 235000013402 health food Nutrition 0.000 claims 1
- 229940079593 drug Drugs 0.000 abstract description 4
- 235000013305 food Nutrition 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000012071 phase Substances 0.000 description 7
- 239000007787 solid Substances 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
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- 230000000694 effects Effects 0.000 description 3
- 239000001963 growth medium Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 238000012258 culturing Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000208421 Ericaceae Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 235000012511 Vaccinium Nutrition 0.000 description 1
- 241000736767 Vaccinium Species 0.000 description 1
- 244000077233 Vaccinium uliginosum Species 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 235000021028 berry Nutrition 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- MGJZITXUQXWAKY-UHFFFAOYSA-N diphenyl-(2,4,6-trinitrophenyl)iminoazanium Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1N=[N+](C=1C=CC=CC=1)C1=CC=CC=C1 MGJZITXUQXWAKY-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000009630 liquid culture Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
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- 239000000523 sample Substances 0.000 description 1
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- 238000007789 sealing Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4973—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
- A61K8/498—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
- A61P39/06—Free radical scavengers or antioxidants
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
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Abstract
The invention discloses a method for extracting anthocyanin from blueberries, and relates to the technical field of anthocyanin extraction. The method comprises the following steps: step 1, mashing blueberries, adding the smashed blueberries into an HCl-ethanol solution, carrying out ultrasonic extraction, carrying out suction filtration, carrying out reduced pressure concentration on an extracting solution, and removing a solvent to obtain a crude extract; step 2, adding the crude extract into a hydrochloric acid aqueous solution for leaching, then adjusting the pH value of the solution and adding ether for extraction, carrying out pressure-reducing concentration on the ether phase, and removing the solvent to obtain an extract A; and 3, adding the extract A into an HCl-ethanol solution for dissolving, adding water for diluting, adding ethyl acetate for extracting, carrying out decompression and concentration on the ethyl acetate, and removing the solvent to obtain the anthocyanin. The method has simple process steps and convenient operation, and is suitable for large-scale industrial production. The anthocyanin extracted by the method has high purity, and can be directly used as a raw material to be added into cosmetics, foods and medicines.
Description
Technical Field
The invention relates to the technical field of anthocyanin extraction, and particularly relates to a method for extracting anthocyanin from blueberries.
Background
Blueberry, also called blueberry, is perennial deciduous leaf or evergreen shrub of Vaccinium (Ericaceae), and the fruit is berry, native to the eastern Canada and the northeast of the United states. The blueberry is rich in anthocyanin, has various pharmacological activities such as antioxidant activity, cancer resistance, vision protection and the like, and has great application potential in the application aspects of food, cosmetics, medicines and the like.
At present, the extraction method of anthocyanin in blueberry mainly comprises an extraction method, an enzymolysis method, an ultrasonic extraction method, a microwave-assisted extraction method and the like, and the extraction method needs to be combined with separation and purification methods such as a macroporous adsorption resin method, a solid phase extraction method, a liquid chromatography method and the like to obtain the anthocyanin with higher purity. The method is complicated in process and is not suitable for large-scale extraction and separation of a large amount of high-purity anthocyanin.
Disclosure of Invention
The invention aims to provide a method for extracting anthocyanin from blueberries, which is used for solving the problems in the prior art and has the characteristics of simple process steps and high extraction efficiency, and the extracted anthocyanin has high purity.
In order to achieve the purpose, the invention provides the following scheme:
the invention discloses a method for extracting anthocyanin from blueberries, which comprises the following steps:
step 1, smashing blueberries, adding the smashed blueberries into an HCl-ethanol solution, carrying out ultrasonic extraction, carrying out suction filtration, carrying out reduced pressure concentration on an extracting solution, and removing a solvent to obtain a crude extract;
step 2, adding the crude extract into a hydrochloric acid aqueous solution for leaching, then adjusting the pH value of the solution to rise, adding ether for extraction, carrying out decompression concentration on the ether, and removing the solvent to obtain an extract A;
and 3, adding the extract A into an HCl-ethanol solution for dissolving, adding water for diluting, then adding ethyl acetate for extracting, carrying out decompression concentration on the ethyl acetate, and removing the solvent to obtain the anthocyanin.
Further, in the step 1, the mass-volume ratio of the blueberries to the HCl-ethanol solution is 1 g; the ultrasonic extraction time is 10-15min.
The ultrasonic extraction time is too short, the anthocyanin cannot be completely dissolved out, the yield of the finally prepared anthocyanin is influenced, the ultrasonic extraction time is too long, the extraction rate is influenced, and therefore, the ultrasonic extraction time is preferably limited to 10-15min.
Further, in the step 2, the pH value of the hydrochloric acid aqueous solution is 3.5-4.0; the leaching temperature is 40-50 deg.C, and the leaching time is 60-80min.
Too low a pH value may destroy the structure of anthocyanin, too high a pH value may affect the leaching rate of anthocyanin, and destroy the structure of anthocyanin, and affect the yield of anthocyanin, therefore, the invention preferably limits the pH of hydrochloric acid aqueous solution to 3.5-4.0.
Too high extraction temperature can destroy the structure of the anthocyanin, and too low extraction temperature can influence the extraction effect of the anthocyanin and influence the yield and purity of the anthocyanin, so that the invention preferably limits the extraction temperature to 40-50 ℃.
Too short leaching time can affect the dissolution effect of anthocyanin in the blueberries, and longer leaching time can affect the extraction speed, so the leaching time is preferably limited to 60-80min.
Further, adjusting the pH value of the solution to be increased to 5-6 in the step 2; the volume ratio of the diethyl ether to the aqueous hydrochloric acid solution is 3:1.
The pH value of the solution is adjusted to be lower than 5, so that the anthocyanin cannot enter the ether phase, and the structure of the anthocyanin is damaged when the pH value is higher than 6, so that the yield and the purity of the anthocyanin are influenced, therefore, the pH value of the solution is preferably adjusted to be 5-6.
Further, in step 3, the volume ratio of the water to the HCl-ethanol solution is 3:1; the volume ratio of the ethyl acetate to the water is 3-5:1.
Further, in step 1 and step 3, the mass percentage of HCl in the HCl-ethanol solution is 1%.
According to the second technical scheme, the anthocyanin is extracted by the extraction method.
In the third technical scheme of the invention, the anthocyanin is applied to preparation of health-care food.
The fourth technical scheme of the invention is the application of the anthocyanin in preparing cosmetics.
The fifth technical scheme of the invention is the application of the anthocyanin in preparing the anti-oxidation, anti-cancer and vision improvement medicines.
The invention discloses the following technical effects:
the method has simple process steps and convenient operation, and is suitable for large-scale industrial production. The anthocyanin extracted by the method has high purity, and can be directly used as a raw material to be added into cosmetics, foods and medicines.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
In the present invention, "%" is calculated by mass percent unless otherwise specified.
The method for detecting the purity of the anthocyanin in the embodiment of the invention is a conventional technical means in the field, does not serve as the key point of the patent protection of the invention, and is not repeated herein.
The blueberries used in the embodiment of the invention are Fenton blueberry.
Example 1
Step 1, adding 10g of mashed blueberries into 30mL1% HCl-ethanol solution, performing ultrasonic extraction for 10min, performing suction filtration, performing reduced pressure concentration on the obtained extracting solution, and removing a solvent to obtain a crude extract;
step 2, dissolving the crude extract prepared in the step 1 in 2 times of hydrochloric acid aqueous solution (pH = 4.0) by mass, leaching for 60min at 40 ℃, adding sodium hydroxide solution to make the pH of the solution 5.0, immediately adding ether with the volume of 3 times of the hydrochloric acid aqueous solution for extraction, carrying out reduced pressure concentration on the ether phase, and removing the solvent to obtain an extract A;
and 3, adding the extract A prepared in the step 2 into a 1-percent HCl-ethanol solution with the mass 2 times of that of the extract A, dissolving the extract A, adding water with the volume 3 times of that of the HCl-ethanol solution into the solution to dilute the solution, adding ethyl acetate with the volume 3 times of that of the solution to extract the solution, repeatedly extracting the solution for 3 times, carrying out reduced pressure concentration on the ethyl acetate, and removing the solvent to obtain 602mg of bluish purple solid, namely the anthocyanin, with the purity of 93.8 percent.
Example 2
Step 1, adding 10g of mashed blueberries into 30mL1 percent of HCl-ethanol solution, performing ultrasonic extraction for 10min, performing suction filtration, concentrating the obtained extracting solution under reduced pressure, and removing a solvent to obtain a crude extract;
step 2, dissolving the crude extract prepared in the step 1 in 2 times of hydrochloric acid aqueous solution (pH = 3.5) by mass, leaching for 60min at 42 ℃, adding sodium hydroxide to make the pH of the solution 5.5, immediately adding ether with the volume 3 times of the hydrochloric acid aqueous solution for extraction, concentrating the ether phase under reduced pressure, and removing the solvent to obtain an extract A;
and 3, adding the extract A prepared in the step 2 into a 1-percent HCl-ethanol solution with the mass 2 times of that of the extract A, dissolving the extract A, adding water with the volume 4 times of that of the 1-percent HCl-ethanol solution to dilute the extract A, adding ethyl acetate with the volume 3 times of that of the extract A to extract the extract A, repeatedly extracting the extract A for 3 times, carrying out reduced pressure concentration on the ethyl acetate phase, and removing the solvent to obtain 571mg of bluish purple solid, namely the anthocyanin with the purity of 94.3 percent.
Example 3
Step 1, adding 10g of mashed blueberries into 30mL1% HCl-ethanol solution, performing ultrasonic extraction for 10min, performing suction filtration, performing reduced pressure concentration on the obtained extracting solution, and removing a solvent to obtain a crude extract;
step 2, dissolving the crude extract prepared in the step 1 in 2 times of hydrochloric acid aqueous solution (pH = 3.8) by mass, leaching for 70min at 45 ℃, adding sodium hydroxide to make the pH of the solution 6.0, immediately adding ether with the volume of 3 times of the hydrochloric acid aqueous solution for extraction, carrying out reduced pressure concentration on the ether phase, and removing the solvent to obtain an extract A;
and 3, adding the extract A prepared in the step 2 into a 1-percent HCl-ethanol solution with the mass 2 times of that of the extract A, dissolving the extract A, adding water with the volume 3 times of that of the 1-percent HCl-ethanol solution, diluting the solution, adding ethyl acetate with the volume 3 times of that of the water, extracting the solution repeatedly for 3 times, carrying out reduced pressure concentration on the ethyl acetate, and removing the solvent to obtain 589mg of bluish purple solid, namely the anthocyanin with the purity of 95.1%.
Example 4
Step 1, adding 10g of mashed blueberries into 25mL1% HCl-ethanol solution, performing ultrasonic extraction for 15min, performing suction filtration, performing reduced pressure concentration on the obtained extracting solution, and removing a solvent to obtain a crude extract;
step 2, dissolving the crude extract prepared in the step 1 in 2 times of hydrochloric acid aqueous solution (pH = 4.0) by mass, leaching for 60min at 50 ℃, adding sodium hydroxide to make the pH of the solution 6.0, immediately adding ether with the volume 3 times of that of the hydrochloric acid aqueous solution for extraction, carrying out reduced pressure concentration on the ether phase, and removing the solvent to obtain an extract A;
step 3, adding the extract a prepared in step 2 to 2-fold mass of 1-fold hcl-ethanol solution for dissolution, adding 3-fold volume of water to the 1-fold hcl-ethanol solution for dilution, adding 3-fold volume of ethyl acetate for extraction, repeating the extraction 3 times, concentrating the ethyl acetate phase under reduced pressure, and removing the solvent to obtain 583mg of bluish-purple solid, namely anthocyanin with a purity of 93.2%.
The antioxidative properties of the anthocyanins prepared in examples 1-4 were measured as follows:
100mg of anthocyanidin was added to 10mL of 1X 10 -4 Adding DPPH solution into mol/L, keeping away from light at room temperature for 90min, measuring the absorbance at the wavelength of 517nm, and recording as A 1 . 0.1mL of distilled water was used instead of anthocyanin to carry out the above operation, and the absorbance was recorded as A 0 . The clearance was calculated as follows:
the results are shown in Table 1.
TABLE 1
| DPPH radical clearance rate | |
| Example 1 | 95％ |
| Example 2 | 97％ |
| Example 3 | 100％ |
| Example 4 | 94％ |
The bacteriostatic effect of the anthocyanins prepared in examples 1-4 was determined as follows:
respectively using inoculating loops to pick out a loop from a strain plate in an ultraclean workbench, streaking the loop on a solid medium plate, marking, and inversely culturing in a biochemical incubator at 37 ℃ for 14h. And (3) selecting two rings of bacterial colonies from the activated escherichia coli and staphylococcus aureus plates, inoculating the two rings of bacterial colonies into 50mL of liquid culture medium, marking, placing in a constant-temperature incubator at 37 ℃, performing shake culture at the rotating speed of 180r/min for 14h until the absorbance of the bacterial colonies reaches 0.8 at the wavelength of 620nm of a spectrophotometer, and stopping culture. The filter paper was punched into a 0.6cm diameter disc with a punch, and the disc was placed in a petri dish and sterilized by sealing. Under aseptic conditions, the filter paper disc was immersed in the sample solution (50 wt% concentration of anthocyanin in ethyl acetate) for 30 minutes with sterile forceps for use. Under aseptic operation, 1mL of seed bacterium liquid is added into every 300mL of sterilized culture medium which is cooled to 55 ℃, the seed bacterium liquid is fully shaken up and poured into a sterile culture dish, after the culture medium is cooled and solidified, a filter paper sheet for soaking samples is placed in a solidified test bacterium flat plate, and two samples are made for each sample in parallel. Standing for 20 minutes, placing the mixture in a constant-temperature incubator at 37 ℃ for culturing for 16 hours, and measuring the size of the inhibition zone. The results are shown in Table 2.
TABLE 2 (units/cm)
| Escherichia coli | Staphylococcus aureus | |
| Example 1 | 3.2 | 3.6 |
| Example 2 | 3.3 | 3.7 |
| Example 3 | 3.5 | 3.9 |
| Example 4 | 3.0 | 3.4 |
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (10)
1. The method for extracting anthocyanin from blueberries is characterized by comprising the following steps:
step 1, mashing blueberries, adding the smashed blueberries into an HCl-ethanol solution, carrying out ultrasonic extraction, carrying out suction filtration, carrying out reduced pressure concentration on an extracting solution, and removing a solvent to obtain a crude extract;
step 2, adding the crude extract into a hydrochloric acid aqueous solution for leaching, then adjusting the pH value of the solution to rise, adding ether for extraction, carrying out decompression concentration on the ether, and removing the solvent to obtain an extract A;
and 3, adding the extract A into an HCl-ethanol solution for dissolving, adding water for diluting, adding ethyl acetate for extracting, carrying out decompression and concentration on the ethyl acetate, and removing the solvent to obtain the anthocyanin.
2. The method for extracting anthocyanin from blueberries according to claim 1, wherein in the step 1, the mass-to-volume ratio of the blueberries to the HCl-ethanol solution is 1g; the ultrasonic extraction time is 10-15min.
3. The method for extracting anthocyanin from blueberries according to claim 1, wherein in the step 2, the pH value of the hydrochloric acid aqueous solution is 3.5-4.0; the leaching temperature is 40-50 deg.C, and the leaching time is 60-80min.
4. The method for extracting anthocyanin in blueberries according to claim 1, wherein in the step 2, the pH value of the solution is adjusted to be increased to 5-6; the volume ratio of the diethyl ether to the hydrochloric acid aqueous solution is 3:1.
5. The method for extracting anthocyanin from blueberries as claimed in claim 1, wherein in the step 3, the volume ratio of the water to the HCl-ethanol solution is 3:1; the volume ratio of the ethyl acetate to the water is 3-5:1.
6. The method for extracting anthocyanin from blueberries according to claim 1, wherein in the step 1 and the step 3, the mass percent of HCl in the HCl-ethanol solution is 1%.
7. The anthocyanin extracted by the extraction method of any one of claims 1 to 6.
8. Use of the anthocyanidin as claimed in claim 7 for the preparation of a health food.
9. Use of the anthocyanidin as claimed in claim 7 for the preparation of cosmetics.
10. The use of the anthocyanins of claim 7 in the preparation of a medicament for anti-oxidant, anti-cancer, and vision improvement.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1613854A (en) * | 2004-08-26 | 2005-05-11 | 上海交通大学 | Extraction of oligomeric anthocyanin from pine bark |
| CN101316831A (en) * | 2005-10-03 | 2008-12-03 | 玛尔斯有限公司 | Process for selectively extracting procyanidins |
| CN101914304A (en) * | 2010-07-30 | 2010-12-15 | 合肥工业大学 | Method for extracting blueberry anthocyanin |
| CN103342692A (en) * | 2013-07-24 | 2013-10-09 | 青岛蓝莓生物科技有限公司 | Method for extracting blueberry anthocyanin |
| CN103626733A (en) * | 2013-11-08 | 2014-03-12 | 天津大学 | Separation method of blueberry anthocyanin |
| CN108059628A (en) * | 2016-11-08 | 2018-05-22 | 中国科学院大连化学物理研究所 | A kind of fast preparation method of blueberry anthocyanin |
| CN112707881A (en) * | 2021-01-22 | 2021-04-27 | 陕西科技大学 | Preparation method of blueberry anthocyanin |
| CN114014830A (en) * | 2021-12-17 | 2022-02-08 | 哈工大机器人南昌智能制造研究院 | Method for producing and preparing blueberry anthocyanin |
-
2022
- 2022-10-20 CN CN202211287651.4A patent/CN115466240A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1613854A (en) * | 2004-08-26 | 2005-05-11 | 上海交通大学 | Extraction of oligomeric anthocyanin from pine bark |
| CN101316831A (en) * | 2005-10-03 | 2008-12-03 | 玛尔斯有限公司 | Process for selectively extracting procyanidins |
| CN101914304A (en) * | 2010-07-30 | 2010-12-15 | 合肥工业大学 | Method for extracting blueberry anthocyanin |
| CN103342692A (en) * | 2013-07-24 | 2013-10-09 | 青岛蓝莓生物科技有限公司 | Method for extracting blueberry anthocyanin |
| CN103626733A (en) * | 2013-11-08 | 2014-03-12 | 天津大学 | Separation method of blueberry anthocyanin |
| CN108059628A (en) * | 2016-11-08 | 2018-05-22 | 中国科学院大连化学物理研究所 | A kind of fast preparation method of blueberry anthocyanin |
| CN112707881A (en) * | 2021-01-22 | 2021-04-27 | 陕西科技大学 | Preparation method of blueberry anthocyanin |
| CN114014830A (en) * | 2021-12-17 | 2022-02-08 | 哈工大机器人南昌智能制造研究院 | Method for producing and preparing blueberry anthocyanin |
Non-Patent Citations (4)
| Title |
|---|
| 徐青 等: "蓝莓花青素的提取及分离研究进展" * |
| 矫馨瑶 等: "蓝莓花青素的研究进展" * |
| 胡雅馨 等: "蓝莓果实中主要营养及花青素成分的研究" * |
| 荆晓艳 等: "葡萄籽原花青素的制备及活性研究" * |
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