CN106810904B - Method for extracting anthocyanin components - Google Patents
Method for extracting anthocyanin components Download PDFInfo
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- CN106810904B CN106810904B CN201710019479.7A CN201710019479A CN106810904B CN 106810904 B CN106810904 B CN 106810904B CN 201710019479 A CN201710019479 A CN 201710019479A CN 106810904 B CN106810904 B CN 106810904B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
Abstract
The invention belongs to the field of natural active substances, and particularly relates to a method for extracting anthocyanin ingredients. A method for extracting anthocyanin ingredients, wherein the method comprises the following steps: 1) extracting the raw material containing anthocyanin ingredients with ethanol, performing alcohol fermentation on the obtained extracting solution, then performing centrifugal filtration, and collecting filtrate; 2) extracting the collected filtrate, and filtering to obtain the anthocyanin component. Compared with the prior art, the extraction method disclosed by the invention not only has high content of the obtained anthocyanin components, but also contains effective components such as mixture alkaloid, superoxide dismutase and the like, has good curative effects on various tumors and various cancers, apoplexy, cardiovascular and cerebrovascular diseases, diabetes, leucoderma, squamous cell disease and cerebral palsy, and can effectively improve and block lymph fluid spread by body fluid, so that cell tumor variation and cancer cell mutation gene variation are caused.
Description
Technical Field
The invention belongs to the technical field of natural active substance extraction, and particularly relates to an extraction method of anthocyanin ingredients.
Background
Anthocyanins (anthocyanidins), also known as anthocyanidins, are water-soluble natural pigments belonging to the class of phenolic flavonoids. Anthocyanin is used as a secondary metabolite in plant bodies and widely exists in plant petals, fruits, leaves and stems, and surface cells of cell sap tissues and stems and leaves of shells of seafood products. The isolated form of anthocyanins under natural conditions is rare and mainly exists in the glycoside form, and more than 250 kinds of naturally occurring anthocyanins are known. The anthocyanin is beneficial to plant pollination and seed propagation, and has the functions of preventing plants from being damaged by ultraviolet irradiation and the like, and meanwhile, the physiological functions of the anthocyanin are widely concerned by researchers at home and abroad, and mainly comprise the aspects of resisting oxidation, removing free radicals, improving immunity, repairing the endogenous function of a human body, tonifying primordial qi, changing acidic constitution, resisting cancer, inhibiting cancer, blocking variant cells, improving the circulatory system, improving the smoothness of skin, protecting the liver, resisting inflammation and bacteria, treating cardiovascular and cerebrovascular diseases, diabetes, vitiligo, psoriasis and the like. In recent years, the research on anthocyanin health-care functions in foreign countries focuses on the aspects of resisting cancers, protecting cardiovascular and beautifying, improving the immunity endogenous function and the like. Therefore, the anthocyanin has wide application prospect in the industries of food, health care products, medicine and the like.
The anthocyanin is usually extracted by adopting a traditional organic solvent, and researches in recent years find that the anthocyanin in the plant is difficult to be fully extracted by simple reagent extraction, and auxiliary methods including microwave, ultrasonic, pressurizing and supercritical CO are gradually developed2Enzyme method, etc. to improve the yield of anthocyanin and shorten the extraction timeIt is good for the quality of extract.
CN103145681A discloses a method for extracting anthocyanidin. The method comprises the following steps: 1) uniformly mixing the raw material containing anthocyanin, split-phase salt, deionized water and a hydrophilic organic solvent, keeping out of the sun, performing aqueous two-phase extraction, and collecting an upper-phase extracting solution; 2) concentrating the upper phase extracting solution obtained in the step 1) to obtain anthocyanin crude extracting solution; 3) adsorbing the crude anthocyanin extract obtained in the step 2) by using a macroporous resin column, washing the macroporous resin with water after the adsorption is saturated, removing impurities until water washing liquid is colorless, eluting with eluent, collecting the eluent, and drying to obtain the anthocyanin.
CN103420970A discloses a method capable of efficiently extracting and purifying anthocyanins, which comprises the following steps: taking squeezed blueberry peels and residues as raw materials, and taking water as an extraction solvent to obtain an extracting solution A; after concentration, adjusting the pH value to acidity to obtain a solution B; separating and purifying by simulated moving bed chromatography to obtain a solution C rich in anthocyanin, and concentrating to obtain a solution D; spray drying to obtain anthocyanin powder. The method adopts a simulated moving bed chromatographic system, and has complex operation and high requirement on equipment.
CN105482493A relates to a method for extracting high-purity anthocyanin. According to the method, purple tomatoes and black nightshade are respectively used as raw materials, firstly smashed and homogenized, mixed with acid water with the pH value of 1, subjected to ultrasonic extraction, filtered, adsorbed by macroporous resin and subjected to impurity removal, then eluted by 95% ethanol with acid with the pH value of 1, and the obtained eluent is subjected to spray drying by a spray dryer to obtain highly purified anthocyanin powder.
CN101999648A discloses a method for extracting anthocyanin and procyanidine components from cranberry fruits, which comprises the following steps: crushing cranberry fruits, performing enzymolysis by using biological enzyme, and performing water extraction under the condition that the pH value is 1.0-5.5 to obtain a water extraction solution and residues; extracting the residue with ethanol, concentrating the extractive solution, and recovering ethanol to obtain ethanol concentrated solution; mixing the water extractive solution and ethanol extractive solution, adsorbing with macroporous adsorbent resin, washing macroporous adsorbent resin with water, resolving with aqueous alcohol solution, concentrating, and drying to obtain mixture containing anthocyanin and procyanidin.
However, the extraction method of the prior art has low extraction rate of anthocyanin components and low content of anthocyanin.
The present invention has been made in view of this situation.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for extracting anthocyanin components, which has high extraction rate of the anthocyanin components and high content of anthocyanin.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for extracting anthocyanin ingredients, wherein the method comprises the following steps:
1) extracting the raw material containing anthocyanin ingredients with ethanol, performing alcohol fermentation on the obtained extracting solution, then performing centrifugal filtration, and collecting filtrate;
2) extracting the collected filtrate, and filtering to obtain the anthocyanin component.
In the above extraction method, the step 1) is: adding 1-3 times of ethanol with the alcohol content of 50-70% for extraction, adding 10-30% of ethanol with the alcohol content into the obtained extracting solution until the alcohol content reaches the alcohol content of 11-65%, standing, centrifuging, filtering, and collecting filtrate.
The extraction method provided by the invention has the advantages that the extraction rate of anthocyanin is high, the anthocyanin content in the extracted anthocyanin component is higher than 90%, the anthocyanin aglycone accounts for more than 80% of the total anthocyanin amount, the bioavailability is higher than 90%, and the anthocyanin has higher medical care value and wider practical application field.
The extraction in the step 1) is carried out for 1-3 times, and the standing is carried out for at least 70 days.
The extraction in the step 2) is carried out according to the following four stages:
1) the first stage is as follows: adding 50-70% alcohol content ethanol into the collected filtrate, soaking at 35 ℃ and 0.4MPa for 48-240 hours, then heating to 45 ℃, and extracting at 0.8MPa for 24-72 hours;
2) and a second stage: cooling to 36 ℃, and extracting for 12-24 hours under the pressure of 0.4 MPa;
3) and a third stage: cooling to-2 ℃, and extracting for 4-8 hours under the pressure of 0.8 MPa; extracting for 4-8 hours under the pressure of 0.4 MPa;
4) a fourth stage: and finally, reducing the temperature from-2 ℃ to-55 ℃, and extracting for 4-12 hours under the pressure of 0.2 MPa.
In the extraction method, the extraction in the step 2) can be carried out for the second extraction and the third extraction … … according to the four stages as required, and the content of the anthocyanin ingredients in the obtained extract is gradually reduced along with the extraction times. After the first extraction, the content of the anthocyanin component is 45-95 percent; after the second extraction, the content of the anthocyanin component is 24-44%; after the third extraction, the content of the anthocyanin component is 6-23%.
The raw material containing anthocyanin ingredients in the step 1) is at least one of blueberry, raspberry, Indian mockstrawberry herb, blackberry, mulberry, honeysuckle fruit, black nightshade fruit, black medlar, cape gooseberry fruit, amur grape, rose, echinacea, common vinca flower, roxburgh rose fruit, lithospermum, purple beet, dendrobium nobile, morning glory, fresh shrimp and shellfish, Chinese magnoliavine fruit, ginseng fruit, pseudo-ginseng fruit, paris polyphylla fruit, acanthopanax fruit and cape gooseberry.
Preferably at least two raw materials of blueberry and roxburgh rose.
The content of SOD superoxide dismutase in the roxburgh rose is 1579-2151 mu g/g, the content of anthocyanin in the fresh blueberry fruit is 163mg/100g, and the anthocyanin can protect a human body from being damaged by free radicals, enhance the elasticity of blood vessels, improve a circulation system, enhance the smoothness of the skin, inhibit inflammation and allergy, improve the flexibility of joints and the like and has a lasting effect. The anthocyanin also has the functions of eliminating eye fatigue, enhancing eyesight, maintaining eye health and preventing eyesight damage, and has the functions of protecting the blood capillaries of eyes so as to promote blood circulation. The blueberry fruit juice beverage preferably contains at least two raw materials of blueberry and roxburgh rose, the extract obtained by the extraction method contains anthocyanin and superoxide dismutase, the effects of the anthocyanin of the blueberry and the SOD of the roxburgh rose can be integrated, and the SOD superoxide dismutase in the roxburgh rose is stable in an acidic environment under the protection of the anthocyanin of the blueberry and has a lasting effect. Meanwhile, when the extract is applied as a health-care product, blueberry anthocyanin is competitively combined with free radicals and oxides in vivo to remove oxygen free radicals in vivo, and the blueberry anthocyanin and rosa roxburghii SOD have mutual protection and promotion effects. Makes up the deficiency of the activity reduction of SOD in an acidic environment, also makes up the deficiency of single health care effect of the existing blueberry product, and is a green, healthy and safe health care product which is easy to be absorbed by human body and has comprehensive nutrition and higher health care value.
As a preferred scheme, the raw materials containing anthocyanin ingredients in step 1) of the invention are a combination of blueberries, raspberries, mock-raspberries, blackberries, mulberries, honeysuckle, black nightshade fruits, black medlars, cape gooseberries, amur grapes, roses, echinacea, vinca minor, rosa roxburghii, lithospermum, purple beets, dendrobium nobile, morning glory, fresh shrimp shells, schisandra chinensis, ginseng fruits, pseudo-ginseng fruits, paris polyphylla fruits, acanthopanax fruits and cape gooseberry fruits.
In the invention, the fresh shrimp and shell comprise 10-35 parts by weight of shrimp heads, 10-60 parts by weight of oyster shells, 10-50 parts by weight of shells and 10-50 parts by weight of concha haliotidis shells.
In the invention, the preferable using amount of other raw material components is as follows: 10-55 parts of blueberry, 10-45 parts of raspberry, 15-45 parts of mock-strawberry, 5-40 parts of blackberry, 5-50 parts of mulberry, 10-55 parts of honeysuckle, 5-50 parts of black nightshade fruit, 5-50 parts of black wolfberry, 5-50 parts of cape gooseberry, 5-50 parts of amur grape, 5-40 parts of rose, 5-50 parts of echinacea, 5-50 parts of small tendril periwinkle, 5-50 parts of roxburgh rose, 5-50 parts of lithospermum, 5-50 parts of purple beet, 5-50 parts of dendrobium devonianum, 5-45 parts of morning glory, 10-70 parts of Chinese magnoliavine fruit, 10-45 parts of ginseng fruit, 10-120 parts of pseudo-ginseng fruit, 5-50 parts of paris polyphylla fruit, 10-50 parts of acanthopanax fruit and 5-50 parts of cape gooseberry.
When the raw material formula is selected, the extract obtained by the extraction method not only contains a plurality of anthocyanin components, but also contains effective components such as mixture alkaloid, superoxide dismutase and the like. Alkaloids: has effects in clearing away heat and toxic materials, expelling pathogenic wind, promoting blood circulation, eliminating phlegm, relieving pain, relieving arthralgia due to wind-dampness, treating pneumonia, asthma, hepatitis, nephritis, and pharyngolaryngitis, promoting blood circulation, dispelling blood stasis, and strengthening tendons and bones. Anthocyanins: has anticancer effect, and can be used for inhibiting tumor, diabetes and heart disease. Superoxide dismutase SOD other mixtures: contains multiple vitamins, trace elements and other unknown effective components, and has obvious effect in inhibiting tumor and cancer cell and leucocyte generation after chemotherapy and radiotherapy. Therefore, the extract obtained by the extraction method has better curative effects on various tumors and cancers, apoplexy, cardiovascular and cerebrovascular diseases, diabetes, leucoderma, squamous cell disease and cerebral palsy, and can effectively improve and block lymph fluid spread by body fluid, thereby causing cell tumor variation and cancer cell mutation gene variation.
The anthocyanin ingredient extracted by the extraction method of the anthocyanin ingredient is applied to the preparation of medicines for treating tumors, cancers, cardiovascular and cerebrovascular diseases, diabetes, leucoderma, squamous cell disease or cerebral palsy, clinical adjuvant therapy functional health-care food, health-care products and health-care drinks containing wine.
In particular, when the anthocyanin compound is used for preparing the medicine for treating tumors, cancers, cardiovascular and cerebrovascular diseases, diabetes, leucoderma, squamous cell disease or cerebral palsy, the content of the anthocyanin compound is 45 to 95 percent.
The anthocyanin ingredients extracted by the extraction method are used for preparing clinical precise innovative treatment medicines for treating tumors, cancers, cardiovascular and cerebrovascular diseases, diabetes, leucoderma, squamous cell disease, cerebral palsy and the like.
When the anthocyanin ingredient is used for preparing clinical adjuvant therapy functional health food and health care products, the content of the anthocyanin ingredient is 24-44%.
When the anthocyanin ingredient is used for preparing the health drink containing wine, the content of the anthocyanin ingredient is 6 to 23 percent.
1) Compared with the prior art, the extraction method disclosed by the invention not only has high content of the obtained anthocyanin components, but also contains effective components such as mixture alkaloid, superoxide dismutase and the like, has good curative effects on various tumors and various cancers, apoplexy, cardiovascular and cerebrovascular diseases, diabetes, leucoderma, squamous cell disease and cerebral palsy, and can effectively improve and block lymph fluid spread by body fluid, so that cell tumor variation and cancer cell mutation gene variation are caused.
2) The extraction method provided by the invention has the advantages that the extraction rate of anthocyanin is high, the anthocyanin content in the extracted anthocyanin component is higher than 90%, the anthocyanin aglycone accounts for more than 80% of the total anthocyanin amount, the bioavailability is higher than 90%, and the anthocyanin has higher medical care value and wider practical application field.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the embodiments of the present invention, and the following embodiments are used for illustrating the present invention and are not intended to limit the scope of the present invention.
Example 1
Consists of the following components: 200kg of blueberries, 200kg of raspberries, 200kg of black nightshade fruits, 200kg of black Chinese wolfberries, 200kg of paris polyphylla fruits, 200kg of Chinese magnoliavine fruits, 200kg of ginseng fruits, 200kg of pseudo-ginseng fruits, 200kg of dendrobium devoninum, 200kg of rosa roxburghii tratt and 200kg of amur grape.
The extraction method comprises the following steps:
1) weighing the raw materials according to the above dosage, mixing, adding 1 time of 50% ethanol for extraction, extracting for 1 time, and mixing extractive solutions; adding 10% ethanol to the extractive solution until the ethanol content reaches 11% ethanol content, standing for 70 days, centrifuging, filtering, and collecting filtrate.
2) Extracting the collected filtrate, and filtering to obtain the anthocyanin component, wherein the extraction is carried out according to the following four stages:
a) the first stage is as follows: adding 50% ethanol into the collected filtrate, soaking at 35 deg.C under 0.4MPa for 48 hr, heating to 45 deg.C, and extracting under 0.8MPa for 24 hr;
b) and a second stage: cooling to 36 deg.C, and extracting under 0.4MPa for 12 hr;
c) and a third stage: cooling to-2 deg.C, and extracting under 0.8MPa for 4 hr; extracting for 4-8 hours under the pressure of 0.4 MPa;
d) a fourth stage: finally, the temperature is reduced from-2 ℃ to-55 ℃, and the extraction is carried out for 4 hours under the pressure of 0.2 MPa.
The anthocyanin component with the total anthocyanin content of 95.13 percent, anthocyanin aglycone accounting for 80.67 percent of the total anthocyanin and the bioavailability of 93.7 percent is obtained, and simultaneously contains alkaloid and superoxide dismutase.
Example 2
Consists of the following components: 300kg of acanthopanax fruit, 300kg of cape gooseberry, 300kg of honeysuckle fruit, 300kg of rose, 300kg of echinacea, 300kg of morning glory, 300kg of vinca minor, 300kg of shrimp head, 300kg of oyster shell, 300kg of abalone shell and 300kg of lithospermum.
The extraction method comprises the following steps:
1) weighing the raw materials according to the above dosage, mixing, adding 3 times of 70% ethanol for extraction for 3 times, and mixing extractive solutions; adding 30% ethanol content ethanol into the extractive solution until the ethanol content reaches 65% ethanol content, standing for 70 days, centrifuging, filtering, and collecting filtrate.
2) Extracting the collected filtrate, and filtering to obtain the anthocyanin component, wherein the extraction is carried out according to the following four stages:
a) the first stage is as follows: adding ethanol with 70% alcohol content into the collected filtrate, soaking at 35 deg.C under 0.4MPa for 240 hr, heating to 45 deg.C, and extracting under 0.8MPa for 72 hr;
b) and a second stage: cooling to 36 deg.C, and extracting under 0.4MPa for 24 hr;
c) and a third stage: cooling to-2 deg.C, and extracting under 0.8MPa for 8 hr; extracting under the pressure of 0.4MPa for 8 hours;
d) a fourth stage: finally, the temperature is reduced from-2 ℃ to-55 ℃, and the extraction is carried out for 12 hours under the pressure of 0.2 MPa.
The anthocyanin component with 95.03% of total anthocyanin content, 80.47% of anthocyanin aglycone in the total anthocyanin content and 92.7% of bioavailability is obtained, and the anthocyanin component also contains alkaloid and superoxide dismutase.
Example 3
Consists of the following components: 400kg of blueberries, 400kg of raspberries, 400kg of black nightshade fruits, 400kg of mulberries, 400kg of rhizoma paridis, 400kg of black Chinese wolfberries, 400kg of blackberries, 400kg of echinacea, 400kg of rosa roxburghii, 400kg of schisandra chinensis, 400kg of Indian mockstrawberry fruits, 400kg of cape jasmine fruits, 400kg of fructus polyporus, 400kg of morning glory, 400kg of roses, 400kg of vinca minor flowers, 400kg of shrimp heads, 400kg of oyster shells, 400kg of concha haliotidis shells, 400kg of lithospermum, 400kg of dendrobium devoninum and 400kg of purple beets.
The extraction method comprises the following steps:
1) weighing the raw materials according to the above dosage, mixing, adding 2 times of 60% ethanol for extraction for 2 times, and mixing extractive solutions; adding ethanol with alcohol content of 20% into the extractive solution until the alcohol content reaches 45% alcohol content, standing for 70 days, centrifuging, filtering, and collecting filtrate.
2) Extracting the collected filtrate, and filtering to obtain the anthocyanin component, wherein the extraction is carried out according to the following four stages:
a) the first stage is as follows: adding 60% ethanol into the collected filtrate, soaking at 35 deg.C under 0.4MPa for 120 hr, heating to 45 deg.C, and extracting under 0.8MPa for 48 hr;
b) and a second stage: cooling to 36 deg.C, and extracting under 0.4MPa for 18 hr;
c) and a third stage: cooling to-2 deg.C, and extracting under 0.8MPa for 6 hr; extracting for 6 hours under the pressure of 0.4 MPa;
d) a fourth stage: finally, the temperature is reduced from-2 ℃ to-55 ℃, and the extraction is carried out for 8 hours under the pressure of 0.2 MPa.
The anthocyanin component with the total anthocyanin content of 94.93 percent, anthocyanin aglycone accounting for 80.37 percent of the total anthocyanin and the bioavailability of 93.5 percent is obtained, and simultaneously contains alkaloid and superoxide dismutase.
Example 4
Consists of the following components: 500kg of blueberries, 500kg of raspberries, 500kg of black nightshade fruits, 500kg of mulberries, 500kg of rhizoma paridis, 500kg of black Chinese wolfberries, 500kg of blackberries, 500kg of echinacea, 500kg of rosa roxburghii, 500kg of schisandra chinensis, 500kg of Indian mockstrawberry fruits, 500kg of cape jasmine fruits, 500kg of fire cagrels, 500kg of morning glory flowers, 500kg of roses, 500kg of vinca minor flowers, 500kg of shrimp heads, 500kg of oyster shells, 500kg of concha haliotidis shells, 500kg of lithospermum, 500kg of dendrobium devonianum, 500kg of purple beet, 500kg of rosa roxburghii and 500.
The extraction method comprises the following steps:
1) weighing the raw materials according to the above dosage, mixing, adding 2 times of 65% ethanol, extracting for 2 times, and mixing extractive solutions; adding ethanol with alcohol content of 20% into the extractive solution until the alcohol content reaches 35% alcohol content, standing for 70 days, centrifuging, filtering, and collecting filtrate.
2) Extracting the collected filtrate, and filtering to obtain the anthocyanin component, wherein the extraction is carried out according to the following four stages:
a) the first stage is as follows: adding 55% ethanol into the collected filtrate, soaking at 35 deg.C under 0.4MPa for 200 hr, heating to 45 deg.C, and extracting under 0.8MPa for 60 hr;
b) and a second stage: cooling to 36 deg.C, and extracting under 0.4MPa for 20 hr;
c) and a third stage: cooling to-2 deg.C, and extracting under 0.8MPa for 5 hr; extracting for 4-8 hours under the pressure of 0.4 MPa;
d) a fourth stage: finally, the temperature is reduced from-2 ℃ to-55 ℃, and the extraction is carried out for 6 hours under the pressure of 0.2 MPa.
The anthocyanin component with the total anthocyanin content of 94.83 percent, anthocyanin aglycone accounting for 80.37 percent of the total anthocyanin and the bioavailability of 93.1 percent is obtained, and the anthocyanin component also contains alkaloid and superoxide dismutase.
Example 5
Consists of the following components: 100kg of blueberries, 100kg of raspberries, 100kg of black nightshade fruits, 100g of mulberries, 100kg of rhizoma paridis, 100kg of black medlar, 100kg of blackberries, 100kg of echinacea, 100kg of rosa roxburghii, 100kg of schisandra chinensis, 100kg of Indian mockstrawberry, 100kg of blackberries, 100kg of cape gooseberry, 100kg of cape jasmine, 100kg of morning glory, 100kg of rose, 100kg of small-vine vinca flowers, 100kg of shrimp heads, 100kg of oyster shells, 100kg of abalone shell shells, 100kg of lithospermum, 100kg of dendrobium devonianum, 100kg of purple beet, 100kg of amur grape and 100kg of rosa roxburghii.
The extraction method comprises the following steps:
1) weighing the raw materials according to the above dosage, mixing, adding 3 times of 55% ethanol, extracting for 2 times, and mixing extractive solutions; adding 28 degree alcohol content ethanol into the extractive solution until the alcohol content reaches 30% alcohol content, standing for 70 days, centrifuging, filtering, and collecting filtrate.
2) Extracting the collected filtrate, and filtering to obtain the anthocyanin component, wherein the extraction is carried out according to the following four stages:
a) the first stage is as follows: adding ethanol with alcohol content of 58% into the collected filtrate, soaking at 35 deg.C under 0.4MPa for 60 hr, heating to 45 deg.C, and extracting under 0.8MPa for 60 hr;
b) and a second stage: cooling to 36 deg.C, and extracting under 0.4MPa for 15 hr;
c) and a third stage: cooling to-2 deg.C, and extracting under 0.8MPa for 6.5 hr; extracting under 0.4MPa for 6.5 hr;
d) a fourth stage: finally, the temperature is reduced from-2 ℃ to-55 ℃, and the extraction is carried out for 10 hours under the pressure of 0.2 MPa.
The anthocyanin component with total anthocyanin content of 95.01%, anthocyanin aglycone accounting for 80.13% of the total anthocyanin and bioavailability of 93.0% is obtained, and the anthocyanin component also contains mixture alkaloid and superoxide dismutase.
Example 6
Weighing 10kg of blueberries and 10kg of roxburgh roses, adding 2 times of 60% alcohol content ethanol for extraction for 2 times, and combining the extracting solutions; adding ethanol with alcohol content of 20% into the extractive solution until the alcohol content reaches 35% alcohol content, standing for 70 days, centrifuging, filtering, and collecting filtrate.
2) Extracting the collected filtrate, and filtering to obtain the anthocyanin component, wherein the extraction is carried out according to the following four stages:
a) the first stage is as follows: adding 60% alcohol content ethanol into the collected filtrate, soaking at 35 deg.C under 0.4MPa for 200 hr, heating to 45 deg.C, and extracting under 0.8MPa for 65 hr;
b) and a second stage: cooling to 36 deg.C, and extracting under 0.4MPa for 20 hr;
c) and a third stage: cooling to-2 deg.C, and extracting under 0.8MPa for 6 hr; extracting for 6 hours under the pressure of 0.4 MPa;
d) a fourth stage: finally, the temperature is reduced from-2 ℃ to-55 ℃, and the extraction is carried out for 10 hours under the pressure of 0.2 MPa.
Example 7
Weighing 10kg of blueberries, adding 2 times of ethanol with the alcohol content of 60 percent for extraction for 2 times, and combining the extracting solutions; adding ethanol with alcohol content of 20% into the extractive solution until the alcohol content reaches 35% alcohol content, standing for 70 days, centrifuging, filtering, and collecting filtrate.
2) Extracting the collected filtrate, and filtering to obtain the anthocyanin component, wherein the extraction is carried out according to the following four stages:
a) the first stage is as follows: adding 60% alcohol content ethanol into the collected filtrate, soaking at 35 deg.C under 0.4MPa for 200 hr, heating to 45 deg.C, and extracting under 0.8MPa for 65 hr;
b) and a second stage: cooling to 36 deg.C, and extracting under 0.4MPa for 20 hr;
c) and a third stage: cooling to-2 deg.C, and extracting under 0.8MPa for 6 hr; extracting for 6 hours under the pressure of 0.4 MPa;
d) a fourth stage: finally, the temperature is reduced from-2 ℃ to-55 ℃, and the extraction is carried out for 10 hours under the pressure of 0.2 MPa.
The extraction efficiency of the blueberry anthocyanin prepared in the embodiment is 95% through detection of a spectrophotometer with the wavelength of 530 nm.
Comparative example 1 extraction of anthocyanidin component according to CN103420970A method
Weighing 10kg of blueberry pericarp and residue, adding 50L of water and 250ml of 10% sulfuric acid solution, extracting at 35 deg.C for 2h, and centrifuging to remove impurities to obtain 45L of extractive solution A. Concentrating the extractive solution A in a concentrator under reduced pressure to 10L containing anthocyanin 1.12g/L, and adding 10% sulfuric acid solution to adjust pH to 1 to obtain solution B. The solution B enters a simulated moving bed chromatogram, an adsorbent is HPD100 macroporous resin, the washing dosage is 1 time of the volume of the resin, and a desorbent is 20% ethanol, the dosage is 2 times of the volume of the resin; the resin regeneration solvent is 95% ethanol; the adsorption flow rate is 1.5 BV/h; the water washing flow rate is 2 BV/h; the elution flow rate is 2 BV/h; the regeneration flow rate is 3 BV/h; the switching time is 800 s; controlling the temperature at 50 ℃; the pressure is controlled at 0.4 MPa. Separating to obtain component solution C rich in anthocyanin, concentrating the solution C to obtain concentrated solution D, and recovering ethanol. And (5) spray drying the concentrated solution D to obtain a product containing anthocyanin.
The extraction efficiency of the blueberry anthocyanin prepared by the comparative example is 86% through the detection of a spectrophotometer with the wavelength of 530 nm.
Test example 1
The products of example 6 and comparative example 1 were tested for anthocyanin content using spectrophotometry:
(1) instruments and reagents: an ultraviolet-visible spectrophotometer; hydrochloric acid methanol solution: adding 5ml of concentrated hydrochloric acid into methanol to 100 ml;
(2) preparation of a sample solution: accurately weighing about 10mg of an anthocyanin sample into a 100ml flask, adding 80ml of hydrochloric acid methanol solution, heating and refluxing for 60min in a water bath at 80 ℃, cooling and transferring into a 100ml volumetric flask, fixing the volume with the hydrochloric acid methanol solution, and absorbing 1ml of hydrochloric acid methanol solution to dilute to 25ml to be used as a sample solution;
(3) and (3) sample determination: the absorbance A was measured at 535nm using a 1cm cuvette blanked with a solution of hydrochloric acid in methanol. The formula is calculated as follows (calculated as delphinidin):
in the formula: a-absorbance of the test sample solution; w is sample weighing, unit g; 1020-absorption coefficient of delphinidin.
The test results are as follows:
| sample (I) | Content of anthocyanidin |
| Example 6 | 91.3％ |
| Comparative example 1 | 66.0％ |
From the test results, the anthocyanin content obtained by the extraction method is high under the condition that the types and the use amounts of the raw materials are the same.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. The extraction method of the anthocyanin components is characterized by comprising the following steps:
1) extracting the raw material containing anthocyanin ingredients with ethanol, performing alcohol fermentation on the obtained extracting solution, then performing centrifugal filtration, and collecting filtrate; the step 1) is as follows: adding 1-3 times of ethanol with the alcohol content of 50-70% for extraction, adding 10-30% of ethanol with the alcohol content into the obtained extracting solution until the alcohol content reaches 11-45% of the alcohol content, standing, carrying out centrifugal filtration, and collecting filtrate, wherein the extraction is carried out for 1-3 times, and the standing is carried out for at least 70 days;
2) extracting the collected filtrate, and filtering to obtain the anthocyanin component; the extraction is carried out according to the following four stages:
1) the first stage is as follows: adding 50-70% ethanol into the collected filtrate, soaking for 48-240 hours at the temperature of 35 ℃ and the pressure of 0.4MPa, then heating to 45 ℃, and extracting for 24-72 hours at the pressure of 0.8 MPa;
2) and a second stage: cooling to 36 ℃, and extracting for 12-24 hours under the pressure of 0.4 MPa;
3) and a third stage: cooling to-2 ℃, and extracting for 4-8 hours under the pressure of 0.8 MPa; extracting for 4-8 hours under the pressure of 0.4 MPa;
4) a fourth stage: and finally, reducing the temperature from-2 ℃ to-55 ℃, and extracting for 4-12 hours under the pressure of 0.2 MPa.
2. The method for extracting anthocyanin-containing ingredients as claimed in claim 1, wherein the raw material containing anthocyanin ingredients in step 1) is at least one of blueberry, raspberry, mock strawberry, blackberry, mulberry, honeysuckle, black nightshade fruit, black wolfberry, cape gooseberry, amur grape, rose, echinacea, vinca minor, roxburgh rose, lithospermum, purple beet, dendrobium nobile, morning glory, schisandra chinensis, ginseng fruit, pseudo-ginseng fruit, paris polyphylla fruit, acanthopanax fruit and cape jasmine fruit.
3. The use of the anthocyanidin component extracted by the extraction method of the anthocyanidin component in claim 1 or 2 in the preparation of drugs for treating tumors, cancers, cardiovascular and cerebrovascular diseases, diabetes, vitiligo, squamous cell disease or cerebral palsy, functional health food for clinical adjuvant therapy, health products and drinks.
4. The use of claim 3, wherein the content of the anthocyanins is 45-95% when the anthocyanins is used for preparing the medicament for treating tumor, cancer, cardiovascular and cerebrovascular diseases, diabetes, vitiligo, squamous cell disease or cerebral palsy.
5. The use of claim 4, wherein the content of the anthocyanins is 24-44% when the anthocyanins is used for preparing clinical adjuvant therapy functional health food and health care products.
6. The use of claim 4, wherein the anthocyanin ingredient is present in an amount of 6% to 23% when the anthocyanin ingredient is used in the preparation of a health beverage containing alcohol.
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