CN110526892B - Method for extracting anthocyanin from blueberry - Google Patents

Method for extracting anthocyanin from blueberry Download PDF

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CN110526892B
CN110526892B CN201910748695.4A CN201910748695A CN110526892B CN 110526892 B CN110526892 B CN 110526892B CN 201910748695 A CN201910748695 A CN 201910748695A CN 110526892 B CN110526892 B CN 110526892B
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leaching
anthocyanin
crystallization
elution
solution
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CN110526892A (en
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何安乐
李伟
黄华学
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Hunan Huacheng Biotech Inc
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Hunan Huacheng Biotech Inc
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic 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
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/58Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
    • C07D311/60Benzo[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
    • C07D311/62Benzo[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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

A method for extracting anthocyanin from indigo honeysuckle comprises the following steps: (1) leaching: leaching the crushed indigo honeysuckle with water as a solvent, and performing solid-liquid separation to obtain a crude extract; (2) and (3) ultrafiltration: ultrafiltering the crude extractive solution, and collecting the filtrate as supernatant; (3) resin adsorption and elution; putting the supernatant on a cation exchange resin column, linearly eluting by adopting a salt solution, collecting the eluate containing anthocyanin, and concentrating to obtain a concentrated solution; (4) and (3) crystallization: adding lower alcohol into the concentrated solution for crystallization, centrifuging, washing and drying to obtain the product after crystallization. The anthocyanin product extracted from the lonicera edulis by the method has high anthocyanin content; and the whole extraction process has the characteristics of mild conditions, high yield, environmental friendliness, suitability for industrial production and the like.

Description

Method for extracting anthocyanin from blueberry
Technical Field
The invention relates to a method for extracting anthocyanin, and in particular relates to a method for extracting anthocyanin from lonicera edulis.
Background
Indigo honeysuckle, also called black wild chrysanthemum, is mainly distributed in Heilongjiang, Jilin and Liaoning places in China, and the taste of the fruit is sweet and sour. Can be used for food, wine and medicine, and is an important wild resource in northeast China. The lonicera caerulea fruit is rich in abundant nutrient substances and also contains a large amount of active anthocyanin, so that relatively few reports and researches on the extraction of the anthocyanin from the lonicera caerulea fruit exist in China at present, and the extraction of the anthocyanin from fresh fruits mainly stays in the processing of fruit wine, fruit juice, jam, preserved fruits and jelly, so that the extraction of the anthocyanin from the lonicera caerulea fruit has a great development prospect.
CN105693680 discloses a method for extracting indigo fruit anthocyanin, which comprises the steps of cleaning raw material indigo fruit, removing impurities, squeezing, separating, acidifying, extracting with ethanol, adsorbing with macroporous resin, desorbing with ethanol, concentrating and drying to obtain the finished product of anthocyanin. The process is simple, the general D101 adsorption resin with wide application range is used, and the obtained product has relatively low anthocyanin content.
CN105884737 discloses a purification process of indigo fruit anthocyanin, which comprises the steps of soaking and crushing in ethanol water solution, homogenizing, solid-liquid separation, macroporous resin adsorption, gradient elution with ethanol water solution, vacuum concentration, and freeze drying to obtain the product. In the method, after leaching, the leaching solution is simply centrifuged and then concentrated to a column, the liquid on the column contains a large amount of non-anthocyanin substances which are easily adsorbed on resin to cause low anthocyanin content of the product, and the used general AB-8 resin has a wide adsorption range and also causes low anthocyanin content of the product.
CN103130762 discloses a method for extracting anthocyanidin from indigo fruit, which comprises soaking and leaching with acidic aqueous solution, adjusting pH, adsorbing with resin, washing with water, eluting with acidic alcohol, concentrating, and drying to obtain anthocyanidin product. The process is simple, and the general D101 adsorption resin with wide application range is used, so that the content of the obtained product is relatively low.
CN105294632 discloses an industrial method for preparing indigo fruit anthocyanin from indigo fruit, which comprises the steps of leaching alkaline aqueous solution containing natural antioxidant, adjusting acid, flocculating, adsorbing by cation exchange resin, eluting by acidic solution, adjusting pH, concentrating under reduced pressure, and spray drying to obtain the product. The process relates to multiple pH adjustment, the anthocyanin is easily degraded, the pH adjustment process is complicated, and the cation exchange resin is eluted by using 2-5% hydrochloric acid subsequently, so that on one hand, the product is easily degraded due to high concentration of hydrochloric acid, and a large amount of chloride ions can be remained in an analytic solution to influence the anthocyanin content and stability of the product.
CN105153739 discloses a preparation method of a blue spindle fruit dye with stable pigment, which comprises stirring in water, crushing, filtering, extracting with absolute ethanol for multiple times, concentrating, adjusting acid, and dissolving with ethanol to obtain the product. The method has simple process, the raw materials are processed into the product, the obtained product has extremely low anthocyanin content, and the product is dye and is only suitable for dyeing textiles.
CN102659870 discloses a method for extracting anthocyanin from indigo fruit, which comprises the steps of juicing and homogenizing through an ethanol water solution, homogenizing, centrifugally separating, concentrating through a thin film, and freeze-drying in vacuum to obtain a product. The method has simple process, and the crude extract of indigo honeysuckle can be obtained by concentrating and drying after extraction, and the anthocyanin content of the product is low.
CN107325139 discloses a method for rapidly and efficiently extracting anthocyanin from indigo honeysuckle, which comprises the steps of homogenizing, crushing, enzymolysis, ethanol extraction, low-temperature ethanol flocculation and sedimentation, reversed-phase column chromatography, methanol elution, concentration and drying to obtain the product. The process utilizes preparative chromatography for chromatographic separation, so that the separation capacity is limited, the treatment efficiency is low, and the amount is small. The subsequent methanol elution may result in excessive methanol residue, and the process is not suitable for industrial production.
CN105885469 discloses a process for extracting anthocyanin from indigo fruit by ultrasonic-microwave synergistic acidified ethanol, which comprises freeze drying, pulverizing, ultrasonic-microwave synergistic acidic ethanol extraction, and centrifuging to obtain anthocyanin extract. The process is simple, and the product content is low, although ultrasonic-microwave synergistic extraction is utilized, the process also stays in the crude extract.
CN106117285 discloses a process for extracting anthocyanin from blueberry by using high-voltage pulse electric field assisted acidified ethanol, which comprises the steps of crushing frozen blueberry, sieving, extracting by using acidified ethanol, treating by using a high-voltage pulse electric field, and carrying out centrifugal separation to obtain an extracting solution. The method is simple, and the obtained product is only crude extract with low anthocyanin content.
CN101463056 discloses a preparation process of macroporous resin purified loniceraedulis anthocyanin, which comprises the steps of drying, crushing, acidified ethanol extraction, rotary evaporation, macroporous resin adsorption, ethanol one-time desorption, concentration and vacuum drying of blueberries to obtain the product. The process involves drying, high temperature can cause target product degradation, single adsorption resin X-5 is used for desorption at one time, and the obtained product has low anthocyanin content.
CN102532219 discloses a method for enriching and purifying anthocyanin in lonicera caerulea, which comprises the steps of raw material crushing, ethanol heating reflux, pressurized ethanol recovery, acid regulation, water washing, macroporous resin adsorption, gradient elution, silica gel column, acetone and methanol solution elution, activated carbon decoloration and recrystallization to obtain the product. The target substance of the primary extract in the method is water-soluble, and the process of washing to be neutral after acid adjustment is difficult to realize; the silica gel column elution uses acetone and methanol, possibly causes residues in subsequent products, and finally uses activated carbon for decolorization and recrystallization, so that the product yield is necessarily low.
CN101434972 discloses a process for preparing loniceraedulis anthocyanin by a solid state biological reaction method, which comprises the steps of crushing pomace under the condition of liquid nitrogen, performing solid state fermentation by xylanase, performing ultrasonic-assisted ethanol extraction, centrifuging to obtain clear liquid, adsorbing by X-5 resin, performing scraper type concentration, and performing vacuum freeze drying to obtain the product. The raw material used by the method is the lonicera edulis pomace, anthocyanin substances of the lonicera edulis pomace are few, and subsequent solid-state fermentation by using xylanase easily causes synchronous fermentation of harmful bacteria so as to metabolize toxic and harmful substances. Compared with the whole process of recycling the pomace waste, the process is complex, the production cost is relatively high, and the process is not suitable for large-scale production.
CN109053834 discloses a method for extracting high-purity cyanidin-3-glucoside from Lonicera caerulea, which comprises grinding frozen fruits, extracting with methanol, centrifuging to obtain supernatant, performing low-temperature rotary concentration, purifying by SPE, eluting with ethyl acetate, eluting with acidic methanol, performing rotary evaporation and filtration membrane, and performing HPLC detection to obtain the product. The method uses methanol for leaching and elution, which can cause methanol residue in the product, and the method uses a C18 column for adsorption, so that the yield is low, the column packing is expensive, the production cost is high, and the large-scale production is difficult.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects and provides a method for extracting anthocyanin from indigo fruit. The method has high yield of the anthocyanin product extracted from the lonicera edulis, high purity of the obtained anthocyanin product and low production cost.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for extracting anthocyanin from indigo honeysuckle comprises the following steps:
(1) leaching: leaching indigo honeysuckle with water as solvent, and performing solid-liquid separation to obtain a crude extract;
(2) and (3) ultrafiltration: ultrafiltering the crude extract obtained in the step (1), and collecting a permeate;
(3) resin adsorption and elution; putting the permeate collected in the step (2) on a cation exchange resin column, linearly eluting by adopting a salt solution, collecting the eluate containing anthocyanin, and concentrating to obtain a concentrated solution;
(4) and (3) crystallization: and adding lower alcohol into the concentrated solution for crystallization, centrifuging, washing and drying after crystallization is finished to obtain the anthocyanin product.
The anthocyanin product extracted from the blueberry has high product content, the whole extraction process has mild conditions, and the method has the characteristics of high yield, environmental friendliness, suitability for industrial production and the like.
Preferably, in the step (1), the leaching temperature is 0-40 ℃, and more preferably, the leaching temperature is 4-20 ℃.
Preferably, in the step (1), the mass ratio of the leached material to water is 1: 20-40, and more preferably, the mass ratio of the material to water is 1: 25-35.
Preferably, in the step (1), the leaching is performed for multiple times, the number of times is 2-5 times, and more preferably, the number of times of leaching is 3-4 times.
Preferably, in the step (1), the leaching time is 3-8 h.
Preferably, in the step (1), the solid-liquid separation mode is that a filter screen is adopted for filtering and centrifugal separation in sequence, the mesh number of the filter screen is 60-200 meshes, and preferably, the mesh number of the filter screen is 100-120 meshes.
Preferably, in the step (1), the centrifugal is a disk-type centrifuge, a horizontal screw-type centrifuge or a three-leg centrifuge.
Preferably, in the step (2), the molecular weight cut-off of the ultrafiltration is 1-20 KDa, and preferably, the molecular weight cut-off of the ultrafiltration is 4-10 KDa.
The ultrafiltration can effectively remove a large amount of macromolecular substances, and is convenient for subsequent column passing, thereby avoiding the column from being blocked.
Preferably, in step (3), the type of the cation exchange resin is selected from one of Dowex-50, D113, D131 or Amberlite IRC-84, and more preferably, the type of the cation exchange resin is Dowex-50.
Preferably, in the step (3), the height-diameter ratio of the cation exchange resin column is 3-10: 1, and more preferably, the height-diameter ratio of the cation exchange resin column is 5-7: 1.
Preferably, in the step (3), the column flow rate of the permeate is 0.3-4 BV/h, and more preferably, the column flow rate of the permeate is 0.5-1.5 BV/h.
A high molecular conjugate system exists in anthocyanin molecules, contains acidic groups, can be adsorbed by cation exchange resin through ion exchange, and the proper height-diameter ratio and sample loading flow rate can fully generate ion exchange, shorten sample loading time and improve column loading efficiency.
Preferably, in the step (3), the salt solution is one or more selected from sodium chloride, potassium chloride, sodium sulfate and potassium sulfate aqueous solution, and more preferably, the salt solution is sodium chloride aqueous solution.
Preferably, in the step (3), the linear elution is performed by starting elution with a salt solution at a concentration of 0M until the concentration of the salt solution is linearly increased to 2.0M, and stopping elution, wherein the volume of the salt solution is 5-10 BV, and the flow rate of the eluent in the linear elution is 0.5-4 BV/h.
Preferably, in the step (3), the linear elution is performed by starting elution with a salt solution at a concentration of 0M until the concentration of the salt solution is linearly increased to 1.0M, and stopping elution, wherein the volume of the salt solution is 6-8 BV, and the flow rate of the eluent in the linear elution is 0.8-2 BV/h.
The sodium chloride is low in price, is suitable for food, is easy to obtain and is particularly suitable for the eluent; the linear elution is more beneficial to eluting ions with different ionic strengths from the resin, so that the separation of the anthocyanin and other impurities is realized.
Preferably, in the step (3), the concentration is performed by using a reverse osmosis membrane until the Brix value of the concentrated solution is 20-60%, and the concentration temperature is not higher than 60 ℃.
Preferably, in the step (3), the concentration is performed by adopting a reverse osmosis membrane until the Brix value of the concentrated solution is 40-50%, and the concentration temperature is not higher than 30 ℃.
Preferably, in the step (4), the lower alcohol is methanol or ethanol, and preferably, the lower alcohol is ethanol.
Preferably, in the step (4), the volume ratio of the lower alcohol to the concentrated solution is 1-20: more preferably, the volume ratio of the lower alcohol to the concentrated solution is 8-15: 1.
preferably, in the step (4), the crystallization temperature is-10 to 40 ℃, the crystallization time is 4 to 24 hours, and more preferably, the crystallization temperature is-4 to 10 ℃, and the crystallization time is 6 to 12 hours.
The growth of the crystal is facilitated by the alcohol solution with proper concentration and low temperature condition, and the crystal growth speed can be accelerated along with stirring.
Preferably, in the step (4), the washing is performed by leaching with the lower alcohol, and the temperature of the washing solution is-10 to 40 ℃.
The washing solution washes the crystals to wash away impurities on the surfaces of the crystals.
Preferably, in the step (4), the drying is vacuum freeze drying, the temperature is-10 to-70 ℃, and the vacuum degree is 5 to 15 Pa.
The vacuum freeze-drying temperature is low, and the influence on anthocyanin is small.
Preferably, in the step (4), the indigo fruit is selected from one or more of fresh indigo fruit, frozen indigo fruit and dehydrated indigo fruit.
Fresh indigo honeysuckle can best keep the anthocyanin from being degraded, while frozen and dehydrated indigo honeysuckle can cause partial degradation of the anthocyanin after processing.
The invention has the beneficial effects that:
(1) the method adopts a linear elution mode to elute the cation exchange resin, so that the target substance is more accurately eluted, and finally, the product is purified again by adopting a crystallization method, so that the content of the anthocyanin in the product is further improved;
(2) the whole extraction process has the advantages of mild conditions, simple process, environmental friendliness and low production cost, and is suitable for industrial production.
Detailed Description
The present invention will be further described with reference to the following examples.
The crushed indigo fruit of the present invention includes fresh indigo fruit, frozen indigo fruit and dehydrated indigo fruit which are subjected to conventional crushing operations such as pressing, grinding and pulverizing.
The method for detecting the content of anthocyanin in the embodiment of the invention is a method for determining a plant extract cowberry fruit extract SW/T-2013 appendix A.2.
The starting materials or chemicals used in the examples of the present invention are, unless otherwise specified, commercially available in a conventional manner.
The cation exchange resin used in the embodiment of the invention is activated before use, and the specific method comprises the following steps: soaking fresh resin in 95% ethanol solution for 24 hr, washing with distilled water until no alcohol smell exists, soaking in 3BV 3.5% NaOH solution for 5.5 hr, washing with distilled water to neutrality, soaking in 3BV 2.5% hydrochloric acid solution for 5.5 hr, and washing with distilled water to neutrality.
The high performance liquid chromatography detector used in the embodiment of the invention is produced by Agilent technologies of Agilent technologies, model number: HPLC-1260.
Example 1
The embodiment comprises the following steps:
(1) leaching: leaching 2000g of fresh indigo honeysuckle (sampling before leaching and inspecting, the mass percentage content of anthocyanin is 0.170%) in cold water at 20 ℃, wherein the amount of the cold water is 30kg, leaching is carried out for 3 times, each time lasts for 8 hours, stirring is carried out discontinuously, after each time of leaching, a 100-mesh filter screen is used for obtaining leaching liquor, and after the leaching liquor is combined, a coarse leaching liquor is obtained after centrifugation;
(2) and (3) ultrafiltration: passing the crude extract obtained in the step (1) through an ultrafiltration membrane with the molecular weight cutoff of 3KDa, and collecting permeate;
(3) resin adsorption: enabling the permeate collected in the step (2) to be nearly saturated through Dowex-50 cation exchange resin with the flow rate of 2BV/h and the high ratio of 8: 1; then, linear elution is carried out on the resin by using a sodium chloride aqueous solution with the concentration of 0-1M from 0M, the elution volume is 10BV, and the elution flow rate is 3 BV/h; after the elution is finished, combining the eluents containing the anthocyanin, and concentrating by using a reverse osmosis membrane until the Brix value is 27 percent and the concentration temperature is not more than 45 ℃;
(4) and (3) crystallization: adding 10 times of 95% methanol into the concentrated solution obtained in the step (3), and then placing the concentrated solution at the temperature of minus 10 ℃ for crystallization for 6 hours with stirring; and after crystallization is finished, centrifugally separating out crystals, then leaching the crystals to be nearly colorless by using methanol with the temperature of minus 10 ℃ and the volume fraction of 95%, and carrying out vacuum freeze drying on the crystals under the conditions of the temperature of minus 20 ℃ and the vacuum degree of 10Pa to obtain 3.54g of anthocyanin products.
Through high performance liquid chromatography detection, the mass percentage content of the anthocyanin in the product obtained in the embodiment is 87.30%, and the yield of the anthocyanin is 90.89%.
Example 2
(1) Leaching: leaching 2000g of frozen lonicera edulis (sampling and inspecting before leaching, the mass percentage content of anthocyanin is 0.165%) in cold water at 10 ℃, wherein the amount of the cold water is 40kg, leaching is carried out for 4 times, each time for 4 hours, stirring is carried out discontinuously, leaching liquor is obtained after each time of leaching through a 100-mesh filter screen, and crude leaching liquor is obtained after merging and centrifuging the leaching liquor;
(2) and (3) ultrafiltration: passing the crude extract obtained in the step (1) through an ultrafiltration membrane with the molecular weight cutoff of 6KDa, and collecting permeate;
(3) resin adsorption: enabling the permeate collected in the step (2) to be nearly saturated through D113 cation exchange resin with the high ratio of 6:1 at the flow rate of 1.5 BV/h; then, linearly eluting the resin from 0M by using a potassium chloride aqueous solution with the concentration of 0-1.5M, wherein the elution volume is 8BV, the elution flow rate is 2BV/h, merging the eluates containing the anthocyanin component after the elution is finished, and concentrating by using a reverse osmosis membrane until the Brix value of the concentrated solution is 48 percent and the concentration temperature is less than or equal to 60 ℃ to obtain a concentrated solution;
(4) and (3) crystallization: adding 28 times of 95% methanol into the concentrated solution obtained in the step (3), then placing the concentrated solution at the temperature of 0 ℃ for crystallization for 12 hours, and stirring the mixture to complete crystallization; centrifuging to separate out crystals, leaching the crystals with methanol with the temperature of 0 ℃ and the volume fraction of 95% until the crystals are nearly colorless, and carrying out vacuum freeze drying at the temperature of minus 60 ℃ and the vacuum degree of 6Pa to obtain 3.64g of anthocyanin product.
Through high performance liquid chromatography detection, the mass percentage of the anthocyanin in the product obtained in the embodiment is 82.46%, and the yield of the anthocyanin is 90.96%.
Example 3
(1) Leaching: 1000g of dehydrated indigo honeysuckle (sampling and inspecting before leaching, the mass percentage content of anthocyanin is 0.270%) is placed in cold water at 4 ℃ for leaching, the dosage of the cold water is 40kg, leaching is carried out for 3 times, each time lasts for 8 hours, and stirring is carried out discontinuously. Leaching with a 100-mesh filter screen to obtain leaching liquor, mixing the leaching liquors, and centrifuging to obtain a crude leaching solution;
(2) and (3) ultrafiltration: passing the crude extract obtained in the step (1) through an ultrafiltration membrane with the molecular weight cutoff of 9KDa, and collecting permeate;
(3) resin adsorption: d131 cation exchange resin with the high ratio of 4:1 at the flow rate of 0.3BV/h is used for the permeate collected in the step (2) until the permeate is nearly saturated; then, linearly eluting the resin from 0M by using a sodium chloride aqueous solution with the concentration of 0-2M, wherein the elution volume is 6BV, the elution flow rate is 1BV/h, combining the eluates containing anthocyanin components after the elution is finished, and concentrating by using a reverse osmosis membrane until the Brix value of the concentrated solution is 59 percent and the concentration temperature is not more than 25 ℃ to obtain a concentrated solution;
(4) and (3) crystallization: and (3) adding 95% ethanol in an amount which is 20 times that of the concentrated solution obtained in the step (3), standing at the temperature of 20 ℃ for crystallization for 20 hours, stirring, centrifuging to separate out crystals after crystallization is completed, leaching the crystals to be nearly colorless by using ethanol with the temperature of 10 ℃ and the volume fraction of 95%, standing the crystals at-350 ℃ and the vacuum degree of 15Pa, and performing vacuum freeze drying to obtain 3.17g of anthocyanin product.
Through high performance liquid chromatography detection, the mass percentage content of the anthocyanin in the product obtained in the embodiment is 79.03%, and the yield of the anthocyanin is 92.79%.

Claims (3)

1. A method for extracting anthocyanin from blueberry is characterized by comprising the following steps:
(1) leaching: leaching the crushed blueberries by using water as a solvent, and carrying out solid-liquid separation to obtain a crude extract; the leaching temperature is 4-20 ℃; the mass ratio of the leached material to water is 1: 20-40; the leaching time is 3-8 h; the leaching is repeated leaching, and the secondary leaching is 2-5 times; the solid-liquid separation mode is that a filter screen is adopted for filtering and centrifugal separation in sequence, and the mesh number of the filter screen is 60-200 meshes;
(2) and (3) ultrafiltration: ultrafiltering the crude extract obtained in the step (1), and collecting a permeate; the cut-off molecular weight of the ultrafiltration is 1-20 KDa;
(3) resin adsorption and elution; putting the permeate collected in the step (2) on a cation exchange resin column, linearly eluting by adopting a salt solution, collecting an eluent containing anthocyanin, and concentrating to obtain a concentrated solution; the type of the cation exchange resin is Dowex-50; the height-diameter ratio of the cation exchange resin column is 3-10: 1; the column feeding flow rate of the permeate liquid is 0.3-4 BV/h; the linear elution refers to that the concentration of a salt solution starts to elute from 0M until the concentration of the salt solution linearly increases to 2.0M, the elution is stopped, the volume of the salt solution is 5-10 BV, and the flow rate of an eluent in the linear elution is 0.5-4 BV/h; the salt solution is sodium chloride aqueous solution; the concentration is carried out by adopting a reverse osmosis membrane until the Brix value of the concentrated solution is 20-60%, and the concentration temperature is less than or equal to 60 ℃;
(4) and (3) crystallization: adding lower alcohol into the concentrated solution obtained in the step (3) for crystallization, and after crystallization is completed, centrifuging, washing and drying to obtain an anthocyanin product; the lower alcohol is methanol; the volume ratio of the lower alcohol to the concentrated solution is 1-20: 1; the crystallization temperature is-10-40 ℃, and the crystallization time is 4-24 h.
2. The method according to claim 1, wherein the mass ratio of the feed to the water is 1: 25-35; the leaching times are 3-4 times.
3. The method of claim 1, wherein the washing is: leaching by using the lower alcohol, wherein the washing temperature is-10-40 ℃; the drying is vacuum freeze drying, the temperature is-10 to-70 ℃, and the vacuum degree is 5 to 15 Pa.
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Citations (2)

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Publication number Priority date Publication date Assignee Title
CN102875514A (en) * 2012-09-25 2013-01-16 凯里学院 Method for extracting and purifying anthocyanins from blueberry red leaves
CN105693680A (en) * 2016-03-22 2016-06-22 吉林省瑞草园科技有限公司 Extraction method of lonicera edulis anthocyanin

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102875514A (en) * 2012-09-25 2013-01-16 凯里学院 Method for extracting and purifying anthocyanins from blueberry red leaves
CN105693680A (en) * 2016-03-22 2016-06-22 吉林省瑞草园科技有限公司 Extraction method of lonicera edulis anthocyanin

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
蓝靛果色素的提取、纯化及性质的研究;扈伊雯;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20170215(第02期);第B024-1235页 *

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