CN114213868A - Method for extracting natural pigment from blueberries - Google Patents

Method for extracting natural pigment from blueberries Download PDF

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Publication number
CN114213868A
CN114213868A CN202210003536.3A CN202210003536A CN114213868A CN 114213868 A CN114213868 A CN 114213868A CN 202210003536 A CN202210003536 A CN 202210003536A CN 114213868 A CN114213868 A CN 114213868A
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Prior art keywords
enzymolysis
blueberry
pigment
jam
solution
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高鸿
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Shaanxi Pioneer Biotech Co ltd
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Shaanxi Pioneer Biotech Co ltd
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Priority to CN202210003536.3A priority Critical patent/CN114213868A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B61/00Dyes of natural origin prepared from natural sources, e.g. vegetable sources
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing 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
    • C09B67/0096Purification; Precipitation; Filtration

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention discloses a method for extracting natural pigment from blueberries, which comprises the following steps: the method comprises the following steps: selecting mature blueberries with complete pericarps; step two: cleaning the selected blueberries in saline water to remove impurities on the skins of the blueberries; step three: putting the washed blueberries into a crusher for crushing to obtain blueberry jam; step four: adding the blueberry jam into an enzymolysis tank, adding a mixed solution of cellulase, hemicellulase, pectinase and papain into the enzymolysis tank for enzymolysis, and obtaining a jam enzymolysis solution after enzymolysis; step five: putting the obtained jam enzymolysis solution into a glass container, adding 60-70% acid ethanol solution into the jam enzymolysis solution to obtain a jam mixed solution, and sealing the glass container; the method for extracting the natural pigment from the blueberries can effectively reduce the difficulty of extracting the natural pigment and improve the purity and the extraction rate of the natural pigment.

Description

Method for extracting natural pigment from blueberries
Technical Field
The invention relates to the technical field of edible pigment preparation, in particular to a method for extracting natural pigment from blueberries.
Background
Blueberry, also known as Vaccinium uliginosum, black bean (great Khingan), Diospyros kaki (great Khingan, Illicun), Diguo, dragon fruit, clam fruit (Jilin), Najasu (Mongolian language), Gieret, Uygur (Orenchun), etc., is a perennial low shrub of Vaccinium of Ericaceae. Native to north america and east asia, distributed in korea, japan, mongolia, russia, europe, north america, black dragon river, inner mongolia, Jilin Changbai mountain and other countries and regions in china, and grown in regions with elevation of 900-2300 m.
The blueberry fruit contains rich nutrient components, especially anthocyanin, and has good nutrition and health care effects, and also has the functions of preventing cranial nerve aging, strengthening heart, resisting cancer, softening blood vessels, enhancing human immunity and the like. The earliest countries for blueberry cultivation were the united states, but the cultivation history to date was less than a hundred years. Because of high health care value, the blueberry pigment is popular in the world, is one of five healthy fruits recommended by food and agricultural organizations in the world, and has low extraction rate, high extraction operation difficulty, low extraction purity and the like when extracting natural pigments from blueberries at present.
Disclosure of Invention
In view of the problems in the prior art, the invention discloses a method for extracting natural pigment from blueberries, which adopts the technical scheme that the method for extracting the natural pigment from the blueberries is characterized by comprising the following steps:
the method comprises the following steps: selecting mature blueberries with complete pericarps;
step two: cleaning the selected blueberries in saline water to remove impurities on the skins of the blueberries;
step three: putting the washed blueberries into a crusher for crushing to obtain blueberry jam;
step four: adding the blueberry jam into an enzymolysis tank, adding a mixed solution of cellulase, hemicellulase, pectinase and papain into the enzymolysis tank for enzymolysis, and obtaining a jam enzymolysis solution after enzymolysis;
step five: putting the obtained jam enzymolysis solution into a glass container, adding an acid ethanol solution with the concentration of 60% into the jam enzymolysis solution to obtain a jam mixed solution, and sealing the glass container;
step six: extracting the jam extract liquid in an ultrasonic extractor, and performing suction filtration on the extracted product to obtain a pigment extract;
step seven: purifying the obtained pigment extract by using a macroporous resin column to obtain a purified blueberry pigment solution;
step eight: filtering the obtained purified blueberry pigment solution through an ultrafiltration membrane, and collecting the intercepted liquid to obtain a blueberry pigment concentrated solution;
step nine: and (4) freeze-drying the blueberry pigment concentrated solution to obtain the blueberry pigment.
As a preferable technical scheme of the invention, the concentration of the brine in the second step is 35-45%.
According to a preferable technical scheme, the mass ratio of the cellulase to the hemicellulase to the pectinase to the papain in the fourth step is 5:2:2: 1.
As a preferred technical scheme of the invention, the enzymolysis temperature in the fourth step is 35-45 ℃, and the enzymolysis time is 6-8H.
As a preferable technical scheme of the invention, the acid ethanol in the step five is a mixed solution of citric acid and ethanol, and the pH value of the mixed solution is 3-4.
As a preferred technical scheme of the invention, the temperature of ultrasonic extraction in the sixth step is 40-50 ℃, and the ultrasonic extraction time is 0.5-1H.
As a preferred technical scheme of the invention, the ultrafiltration membrane in the step eight has the molecular weight cut-off of 400-500 Da.
As a preferable technical scheme of the invention, the temperature of the freeze drying in the ninth step is-30 ℃ to-50 ℃.
The invention has the beneficial effects that: the invention adopts a solvent method to extract the pigment, and adopts an enzymolysis method and an ultrasonic method to extract the natural pigment in the blueberries, thereby effectively reducing the difficulty of extracting the natural pigment and improving the purity and the extraction rate of the natural pigment.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
Example 1
As shown in figure 1, the invention discloses a method for extracting natural pigment from blueberries, which adopts the technical scheme that the method comprises the following steps:
the method comprises the following steps: selecting mature blueberries with complete pericarps;
step two: cleaning the selected blueberries in saline water to remove impurities on the skins of the blueberries;
step three: putting the washed blueberries into a crusher for crushing to obtain blueberry jam;
step four: adding the blueberry jam into an enzymolysis tank, adding a mixed solution of cellulase, hemicellulase, pectinase and papain into the enzymolysis tank for enzymolysis, and obtaining a jam enzymolysis solution after enzymolysis;
step five: putting the obtained jam enzymolysis solution into a glass container, adding 60-70% acid ethanol solution into the jam enzymolysis solution to obtain a jam mixed solution, and sealing the glass container;
step six: extracting the jam extract liquid in an ultrasonic extractor, and performing suction filtration on the extracted product to obtain a pigment extract;
step seven: purifying the obtained pigment extract by using a macroporous resin column to obtain a purified blueberry pigment solution;
step eight: filtering the obtained purified blueberry pigment solution through an ultrafiltration membrane, and collecting the intercepted liquid to obtain a blueberry pigment concentrated solution;
step nine: and (4) freeze-drying the blueberry pigment concentrated solution to obtain the blueberry pigment.
In a preferred embodiment of the present invention, the brine concentration in the second step is 35%.
According to a preferable technical scheme, the mass ratio of the cellulase to the hemicellulase to the pectinase to the papain in the fourth step is 5:2:2: 1.
As a preferred technical scheme of the invention, the enzymolysis temperature in the fourth step is 35 ℃, and the enzymolysis time is 6H.
In a preferred embodiment of the present invention, the acid ethanol in the step five is a mixed solution of citric acid and ethanol, and the PH value of the mixed solution is 3.
As a preferable technical scheme of the invention, the temperature of ultrasonic extraction in the sixth step is 40 ℃, and the ultrasonic extraction time is 0.5H.
As a preferred technical scheme of the invention, the ultrafiltration membrane in the step eight has the molecular weight cut-off of 400 Da.
As a preferred technical scheme of the invention, the temperature of freeze drying in the ninth step is-30 ℃.
Example 2
As shown in figure 1, the invention discloses a method for extracting natural pigment from blueberries, which adopts the technical scheme that the method comprises the following steps: selecting mature blueberries with complete pericarps;
step two: cleaning the selected blueberries in saline water to remove impurities on the skins of the blueberries;
step three: putting the washed blueberries into a crusher for crushing to obtain blueberry jam;
step four: adding the blueberry jam into an enzymolysis tank, adding a mixed solution of cellulase, hemicellulase, pectinase and papain into the enzymolysis tank for enzymolysis, and obtaining a jam enzymolysis solution after enzymolysis;
step five: putting the obtained jam enzymolysis solution into a glass container, adding 65% acid ethanol solution into the jam enzymolysis solution to obtain a jam mixed solution, and sealing the glass container;
step six: extracting the jam extract liquid in an ultrasonic extractor, and performing suction filtration on the extracted product to obtain a pigment extract;
step seven: purifying the obtained pigment extract by using a macroporous resin column to obtain a purified blueberry pigment solution;
step eight: filtering the obtained purified blueberry pigment solution through an ultrafiltration membrane, and collecting the intercepted liquid to obtain a blueberry pigment concentrated solution;
step nine: and (4) freeze-drying the blueberry pigment concentrated solution to obtain the blueberry pigment.
In a preferred embodiment of the present invention, the brine concentration in the second step is 40%.
According to a preferable technical scheme, the mass ratio of the cellulase to the hemicellulase to the pectinase to the papain in the fourth step is 5:2:2: 1.
As a preferred technical scheme of the invention, the enzymolysis temperature in the fourth step is 40 ℃, and the enzymolysis time is 7H.
In a preferred embodiment of the present invention, the acid ethanol in the step five is a mixed solution of citric acid and ethanol, and the PH value of the mixed solution is 3.5.
As a preferable technical scheme of the invention, the temperature of ultrasonic extraction in the sixth step is 45 ℃, and the ultrasonic extraction time is 0.75H.
In a preferred embodiment of the present invention, the ultrafiltration membrane in step eight has a molecular weight cut-off of 450 Da.
As a preferred technical scheme of the invention, the temperature of freeze drying in the ninth step is-45 ℃.
Example 3
As shown in figure 1, the invention discloses a method for extracting natural pigment from blueberries, which adopts the technical scheme that the method comprises the following steps:
the method comprises the following steps: selecting mature blueberries with complete pericarps;
step two: cleaning the selected blueberries in saline water to remove impurities on the skins of the blueberries;
step three: putting the washed blueberries into a crusher for crushing to obtain blueberry jam;
step four: adding the blueberry jam into an enzymolysis tank, adding a mixed solution of cellulase, hemicellulase, pectinase and papain into the enzymolysis tank for enzymolysis, and obtaining a jam enzymolysis solution after enzymolysis;
step five: putting the obtained jam enzymolysis solution into a glass container, adding 70% acid ethanol solution into the jam enzymolysis solution to obtain a jam mixed solution, and sealing the glass container;
step six: extracting the jam extract liquid in an ultrasonic extractor, and performing suction filtration on the extracted product to obtain a pigment extract;
step seven: purifying the obtained pigment extract by using a macroporous resin column to obtain a purified blueberry pigment solution;
step eight: filtering the obtained purified blueberry pigment solution through an ultrafiltration membrane, and collecting the intercepted liquid to obtain a blueberry pigment concentrated solution;
step nine: and (4) freeze-drying the blueberry pigment concentrated solution to obtain the blueberry pigment.
In a preferred embodiment of the present invention, the brine concentration in the second step is 45%.
According to a preferable technical scheme, the mass ratio of the cellulase to the hemicellulase to the pectinase to the papain in the fourth step is 5:2:2: 1.
As a preferred technical scheme of the invention, the enzymolysis temperature in the fourth step is 45 ℃, and the enzymolysis time is 8H.
In a preferred embodiment of the present invention, the acid ethanol in the step five is a mixed solution of citric acid and ethanol, and the PH value of the mixed solution is 4.
As a preferable technical scheme of the invention, the temperature of ultrasonic extraction in the sixth step is 50 ℃, and the ultrasonic extraction time is 0.1H.
As a preferred technical scheme of the invention, the ultrafiltration membrane in the step eight has the molecular weight cut-off of 500 Da.
As a preferable technical scheme of the invention, the temperature of the freeze drying in the ninth step is-30 ℃ to-50 ℃.
The working principle of the invention is as follows: selecting mature blueberries with complete pericarps; cleaning the selected blueberries in saline water to remove impurities on the skins of the blueberries; putting the washed blueberries into a crusher for crushing to obtain blueberry jam; adding the blueberry jam into an enzymolysis tank, adding a mixed solution of cellulase, hemicellulase, pectinase and papain into the enzymolysis tank for enzymolysis, and obtaining a jam enzymolysis solution after enzymolysis; putting the obtained jam enzymolysis solution into a glass container, adding an acid ethanol solution into the jam enzymolysis solution to obtain a jam mixed solution, and sealing the glass container; extracting the jam extract liquid in an ultrasonic extractor, and performing suction filtration on the extracted product to obtain a pigment extract; purifying the obtained pigment extract by using a macroporous resin column to obtain a purified blueberry pigment solution; filtering the obtained purified blueberry pigment solution through an ultrafiltration membrane, and collecting the intercepted liquid to obtain a blueberry pigment concentrated solution; the blueberry pigment concentrated solution is freeze-dried to obtain the blueberry pigment, natural pigments in blueberries are extracted by a plurality of methods, the difficulty of extracting the natural pigments can be effectively reduced, and the purity and the extraction rate of the natural pigments are improved.
Parts not described in detail herein are prior art.
Although the present invention has been described in detail with reference to the specific embodiments, the present invention is not limited to the above embodiments, and various changes and modifications without inventive changes may be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.

Claims (8)

1. A method for extracting natural pigment from blueberries is characterized by comprising the following steps:
the method comprises the following steps: selecting mature blueberries with complete pericarps;
step two: cleaning the selected blueberries in saline water to remove impurities on the skins of the blueberries;
step three: putting the washed blueberries into a crusher for crushing to obtain blueberry jam;
step four: adding the blueberry jam into an enzymolysis tank, adding a mixed solution of cellulase, hemicellulase, pectinase and papain into the enzymolysis tank for enzymolysis, and obtaining a jam enzymolysis solution after enzymolysis;
step five: putting the obtained jam enzymolysis solution into a glass container, adding 60-70% acid ethanol solution into the jam enzymolysis solution to obtain a jam mixed solution, and sealing the glass container;
step six: extracting the jam extract liquid in an ultrasonic extractor, and performing suction filtration on the extracted product to obtain a pigment extract;
step seven: purifying the obtained pigment extract by using a macroporous resin column to obtain a purified blueberry pigment solution;
step eight: filtering the obtained purified blueberry pigment solution through an ultrafiltration membrane, and collecting the intercepted liquid to obtain a blueberry pigment concentrated solution;
step nine: and (4) freeze-drying the blueberry pigment concentrated solution to obtain the blueberry pigment.
2. The method for extracting natural pigment from blueberry according to claim 1, which is characterized in that: and the concentration of the brine in the second step is 35-45%.
3. The method for extracting natural pigment from blueberry according to claim 1, which is characterized in that: the mass ratio of the cellulase to the hemicellulase to the pectinase to the papain in the fourth step is 5:2:2: 1.
4. The method for extracting natural pigment from blueberry according to claim 1, which is characterized in that: in the fourth step, the enzymolysis temperature is 35-45 ℃, and the enzymolysis time is 6-8H.
5. The method for extracting natural pigment from blueberry according to claim 1, which is characterized in that: and the acid ethanol in the step five is a mixed solution of citric acid and ethanol, and the pH value of the acid ethanol is 3-4.
6. The method for extracting natural pigment from blueberry according to claim 1, which is characterized in that: in the sixth step, the ultrasonic extraction temperature is 40-50 ℃, and the ultrasonic extraction time is 0.5-1H.
7. The method for extracting natural pigment from blueberry according to claim 1, which is characterized in that: the molecular weight cut-off of the ultrafiltration membrane in the step eight is 400-500 Da.
8. The method for extracting natural pigment from blueberry according to claim 1, which is characterized in that: the temperature of the freeze drying in the ninth step is-30 ℃ to-50 ℃.
CN202210003536.3A 2022-01-05 2022-01-05 Method for extracting natural pigment from blueberries Pending CN114213868A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2285708C1 (en) * 2005-12-15 2006-10-20 Государственное образовательное учреждение высшего профессионального образования "Московский государственный университет пищевых производств" Министерства образования Российской Федерации Method for production of natural food grade colorant from plant raw materials and waste from plant raw material processing, and obtained natural food grade colorant
KR20140063296A (en) * 2012-11-16 2014-05-27 단국대학교 산학협력단 Method for preparation of extracts of berries and colored potatos comprising anthocyanin-based pigments using pectinex ultra sp-l
CN105949166A (en) * 2016-07-13 2016-09-21 吉林省普蓝高科技有限公司 Extraction method for blueberry anthocyanin
CN108727328A (en) * 2018-08-10 2018-11-02 合肥师范学院 A kind of high efficiency extraction and purification process of blueberry anthocyanin
CN111978280A (en) * 2020-09-04 2020-11-24 中国药科大学 Extraction, separation and purification method of blueberry anthocyanin

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2285708C1 (en) * 2005-12-15 2006-10-20 Государственное образовательное учреждение высшего профессионального образования "Московский государственный университет пищевых производств" Министерства образования Российской Федерации Method for production of natural food grade colorant from plant raw materials and waste from plant raw material processing, and obtained natural food grade colorant
KR20140063296A (en) * 2012-11-16 2014-05-27 단국대학교 산학협력단 Method for preparation of extracts of berries and colored potatos comprising anthocyanin-based pigments using pectinex ultra sp-l
CN105949166A (en) * 2016-07-13 2016-09-21 吉林省普蓝高科技有限公司 Extraction method for blueberry anthocyanin
CN108727328A (en) * 2018-08-10 2018-11-02 合肥师范学院 A kind of high efficiency extraction and purification process of blueberry anthocyanin
CN111978280A (en) * 2020-09-04 2020-11-24 中国药科大学 Extraction, separation and purification method of blueberry anthocyanin

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
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