CN110938054A - Method for preparing indigo fruit anthocyanin from indigo fruit - Google Patents
Method for preparing indigo fruit anthocyanin from indigo fruit Download PDFInfo
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- CN110938054A CN110938054A CN201811110903.XA CN201811110903A CN110938054A CN 110938054 A CN110938054 A CN 110938054A CN 201811110903 A CN201811110903 A CN 201811110903A CN 110938054 A CN110938054 A CN 110938054A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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- 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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Abstract
The invention discloses a method for preparing lonicera edulis anthocyanin from lonicera edulis, which comprises the following steps: crushing and pulping fresh lonicera edulis by adopting a colloid mill, extracting the lonicera edulis by utilizing a subcritical water extraction technology in the presence of an antioxidant, centrifuging, placing the centrifugate to room temperature for layering, collecting a lower water layer, filtering the water layer, winterizing and filtering, treating the filtrate by adopting a ceramic membrane and a nanofiltration membrane in sequence, and finally adopting molecular distillation and vacuum freeze-drying technologies to obtain a lonicera edulis anthocyanin finished product. The lonicera edulis anthocyanin product prepared by the method has the advantages of no solvent residue, low cost, no environmental pollution, high use and edible safety and the like.
Description
Technical Field
The invention belongs to the field of natural organic chemistry, and relates to a method for preparing lonicera edulis anthocyanin by taking lonicera edulis as a raw material. In particular to a method for preparing lonicera edulis anthocyanin by utilizing subcritical water technology extraction, winterization and membrane technology purification.
Background
Anthocyanidin is a water-soluble pigment, and can change color with acid and alkali of cell sap. The acid cell sap is reddish, the alkaline cell sap is blue, and anthocyanin is one of the main pigments forming the colors of petals and fruits. The anthocyanin is a plant secondary metabolite and plays an important role in physiology, is a pure natural anti-aging nutritional supplement, is one of the most effective plant antioxidants found by human beings at present, has the biological effectiveness of 100 percent on a human body, can be detected in blood twenty minutes after being taken, has obvious effects of enhancing eyesight, eliminating eye fatigue and delaying cranial nerve aging, has a better treatment effect on capillary diseases caused by diabetes, and also can enhance the functions of heart and lung and prevent senile dementia and other diseases.
The lonicera edulis is a fruit of lonicera japonica of the genus lonicera of the family loniceraceae, is an oval bluish purple berry, contains a large amount of anthocyanin, mainly contains anthocyanin substances taking cyanidin as a main component and anthocyanin substances taking cyanidin as an aglycon, and is one of the plant sources containing much anthocyanin at present.
The current common extraction methods for preparing anthocyanin are as follows: organic solvent extraction, supercritical extraction, microwave extraction and ultrasonic extraction. Organic solvent extraction is a common method for extracting anthocyanin, and after extraction with a solvent, some organic solvents such as petroleum ether, n-hexylen, diethyl ether and the like are required for extraction to remove fat-soluble substances in a crude extract. The organic solvent extraction method has the advantages of simple extraction equipment and simple and convenient operation; the disadvantages are that the organic solvent is easy to consume, takes time, easily causes high solvent residue in the product, and also causes pollution to the environment. The microwave method and the ultrasonic method may cause great harm to the health of operators due to equipment factors. The supercritical extraction method can realize industrialization at present, but as the technology is to convert gaseous carbon dioxide into liquid carbon dioxide, and the liquid carbon dioxide has stronger extraction capability on fat-soluble substances, the proportion of fat-soluble impurities in the product is higher, thereby greatly increasing the cost for producing the anthocyanin.
The prior common purification method is mainly carried out by adopting macroporous adsorption resin, and the macroporous adsorption resin has the advantages of large adsorption capacity and repeated utilization; the disadvantages are that a large amount of ethanol is needed for elution in the purification process, the loss amount of the solvent is large, and the production cost is increased.
Disclosure of Invention
The invention aims to provide a preparation method of anthocyanin in lonicera edulis. The lonicera edulis anthocyanin product is obtained by pulping lonicera edulis, extracting by using subcritical water, enriching by using winterization and membrane technology, and finally performing molecular distillation and freeze drying.
The technical scheme of the invention is realized in such a way that the method comprises the following steps:
(1) crushing and pulping fresh indigo honeysuckle fruits by adopting a colloid mill to obtain fruit pulp;
(2) extracting the fruit pulp obtained in the step (1) by using a subcritical water extraction technology in the presence of an antioxidant;
(3) introducing the feed liquid extracted in the step (2) into a centrifuge for centrifugation, and collecting a centrifugate;
(4) standing the centrifugate obtained in the step (3) to room temperature for layering, collecting a lower water layer, and filtering the water layer to obtain a filtrate A;
(5) winterizing the filtrate A in the step (4), and then filtering again to obtain a filtrate B;
(6) treating the filtrate B in the step (5) by adopting a ceramic membrane and a nanofiltration membrane in sequence to obtain a concentrated solution A;
(7) concentrating the concentrated solution A in the step (6) by adopting molecular distillation to obtain a concentrated solution B;
(8) and (5) carrying out vacuum freeze drying on the concentrated solution B in the step (7) to obtain finished product powder containing the lonicera edulis anthocyanin.
The better technical scheme of the invention is as follows: in the step (2), the indigo fruit pulp is extracted by adopting a subcritical water extraction technology, the pressure range is 16-20 MPa, the extraction temperature is 300-340 ℃, and the fruit pulp: water =1: 1-3 (m/m), extraction time is 10-30 min, and extraction is performed for 2 times.
The better technical scheme of the invention is as follows: in the step (2), the added antioxidant is EGCG, and the addition amount of the 2 times of extraction is 0.01-0.05% of the weight of the lonicera edulis.
The better technical scheme of the invention is as follows: in the step (5), the winterization temperature is 1-5 ℃, and the winterization time is 5-10 h.
The better technical scheme of the invention is as follows: in the step (6), a membrane element with the aperture of 200nm is selected as the aperture of the ceramic membrane, the temperature of the ceramic membrane treatment solution is 21-25 ℃, and the pressure is 0.2-0.4 MPa; the molecular weight cut-off of the nanofiltration membrane is 200-400 Da, the temperature of the nanofiltration membrane treatment liquid is 23-28 ℃, and the pressure is 0.3-0.5 MPa.
The better technical scheme of the invention is as follows: in the step (7), the pressure of molecular distillation is 20-30 Pa, the evaporation temperature is 30-35 ℃, the condensation temperature is 0-10 ℃, and the material flow rate is 1.0-2.0L/min.
The better technical scheme of the invention is as follows: in the step (8), the vacuum degree is controlled to be 10-13 Pa during freezing, the temperature is controlled to be-50 to-40 ℃, and the freezing and drying are carried out until the moisture content is below 5 percent.
The invention has the following advantages:
1. according to the method, the lonicera edulis is pulped by adopting the colloid mill, so that the contact area of the raw materials and water in the extraction process can be effectively increased, and the extraction yield is improved.
2. The invention adopts subcritical water extraction technology, adopts water in a subcritical state as an extraction solvent instead of other organic solvents and acidic aqueous solutions, can improve extraction efficiency, avoids resource waste, does not pollute the environment, does not have solvent residue in products, and greatly improves the use and edible safety of anthocyanin.
3. In the subcritical water extraction process, the antioxidant is added, so that the influence of the extraction temperature on the anthocyanin can be effectively reduced, and the loss of the anthocyanin is reduced.
4. Compared with other purification processes requiring organic solvents, the method for enriching anthocyanin by adopting winterization and membrane technology has the advantages of simple operation, resource saving, no environmental pollution, no introduction of organic solvents into products and the like.
Detailed description of the preferred embodiments
Example 1
Crushing and pulping 1kg of fresh indigo honeysuckle in a colloid mill, adding 1kg of purified water, stirring uniformly, and extracting for 30min under the conditions of 16Mpa of pressure and 300 ℃. And (3) centrifuging the feed liquid by using a centrifuge after extraction is finished, collecting the centrifugate to a storage tank, and extracting the material slag for the 2 nd time. The weight of EGCG added in each extraction was 0.4 g. Mixing the extractive solutions for 2 times, standing at room temperature for layering, discharging lower water layer, filtering the water layer to obtain filtrate A, winterizing filtrate A in 2 deg.C refrigerator for 6 hr, and filtering again to obtain 2.63kg filtrate B.
And finely filtering the filtrate B by adopting a ceramic membrane, wherein a membrane element with the aperture of 200nm is selected as the ceramic membrane, the temperature of the treatment solution is 21 ℃, the pressure is 0.4MPa, and collecting the ceramic membrane permeate. And concentrating the ceramic membrane permeate by using a nanofiltration membrane, wherein the cut-off molecular weight of the nanofiltration membrane is 200-400 Da, the temperature of the treatment solution is 23 ℃, and the pressure is 0.5 MPa. Purified water was repeatedly added to the concentrated solution, and the resulting solution was passed through a nanofiltration membrane to transfer the anthocyanins to the concentrated solution a as much as possible, thereby obtaining 3.01kg of the concentrated solution a.
Distilling the concentrated solution A by using molecular distillation equipment, wherein the pressure of molecular distillation is 20Pa, the evaporation temperature is 30 ℃, the condensation temperature is 0 ℃, and the material flow rate is 1.0L/min, so as to obtain 263.2g of molecular distillation concentrated solution B. And finally, putting the molecular distillation concentrated solution B into a vacuum freeze dryer for drying, controlling the vacuum degree to be 10Pa and the temperature to be-50 ℃, and freeze-drying until the water content is 4.53%. The obtained indigo fruit anthocyanin has weight of 51.2g, wherein the purity of the anthocyanin is 21.24%.
Example 2
Crushing and pulping 1kg of fresh indigo honeysuckle in a colloid mill, adding 2kg of purified water, stirring uniformly, and extracting for 20min under the conditions that the pressure is 18Mpa and the temperature is 320 ℃. And (3) centrifuging the feed liquid by using a centrifuge after extraction is finished, collecting the centrifugate to a storage tank, and extracting the material slag for the 2 nd time. The weight of EGCG added in each extraction was 0.3 g. Mixing the extractive solutions for 2 times, standing at room temperature for layering, discharging lower water layer, filtering the water layer to obtain filtrate A, winterizing the filtrate A in a refrigerator at 5 deg.C for 8 hr, and filtering again to obtain 4.61kg filtrate B.
And finely filtering the filtrate B by adopting a ceramic membrane, wherein a membrane element with the aperture of 200nm is selected as the ceramic membrane, the temperature of the treatment solution is 23 ℃, the pressure is 0.3MPa, and collecting the ceramic membrane permeate. And concentrating the ceramic membrane permeate by using a nanofiltration membrane, wherein the cut-off molecular weight of the nanofiltration membrane is 200-400 Da, the temperature of the treatment solution is 25 ℃, and the pressure is 0.4 MPa. Purified water was repeatedly added to the concentrated solution, and the resulting solution was passed through a nanofiltration membrane to transfer anthocyanins to the concentrated solution a as much as possible, thereby obtaining 4.73kg of the concentrated solution a.
Distilling the concentrated solution A by using molecular distillation equipment, wherein the pressure of molecular distillation is 30Pa, the evaporation temperature is 35 ℃, the condensation temperature is 10 ℃, and the material flow rate is 2.0L/min, so that 277.1g of molecular distillation concentrated solution B is obtained. And finally, putting the molecular distillation concentrated solution B into a vacuum freeze dryer for drying, controlling the vacuum degree to be 13Pa and the temperature to be-40 ℃, and freeze-drying until the water content is 4.69%. The obtained indigo fruit anthocyanin has a weight of 52.3g, wherein the purity of the anthocyanin is 20.73%.
Example 3
Crushing and pulping 1kg of fresh indigo honeysuckle in a colloid mill, adding 3kg of purified water, stirring uniformly, and extracting for 15min under the conditions that the pressure is 20Mpa and the temperature is 340 ℃. And (3) centrifuging the feed liquid by using a centrifuge after extraction is finished, collecting the centrifugate to a storage tank, and extracting the material slag for the 2 nd time. The weight of EGCG added in each extraction was 0.5 g. Mixing the extractive solutions for 2 times, standing at room temperature for layering, discharging lower water layer, filtering the water layer to obtain filtrate A, winterizing the filtrate A in 1 deg.C refrigerator for 10 hr, and filtering again to obtain 6.58kg filtrate B.
And finely filtering the filtrate B by adopting a ceramic membrane, wherein a membrane element with the aperture of 200nm is selected as the ceramic membrane, and the ceramic membrane permeate is collected at the temperature of 25 ℃ and the pressure of 0.2 MPa. And concentrating the ceramic membrane permeate by using a nanofiltration membrane, wherein the cut-off molecular weight of the nanofiltration membrane is 200-400 Da, the temperature of the treatment solution is 28 ℃, and the pressure is 0.3 MPa. Purified water was added to the concentrated solution, and the resulting solution was passed through a nanofiltration membrane to transfer anthocyanins to the concentrated solution a as much as possible, thereby obtaining 6.66kg of the concentrated solution a.
Distilling the concentrated solution A by using molecular distillation equipment, wherein the pressure of molecular distillation is 25Pa, the evaporation temperature is 33 ℃, the condensation temperature is 4 ℃, and the material flow rate is 1.5L/min, so as to obtain 258.4g of molecular distillation concentrated solution B. And finally, putting the molecular distillation concentrated solution B into a vacuum freeze dryer for drying, controlling the vacuum degree to be 13Pa and the temperature to be-50 ℃, and freeze-drying until the water content is 4.47%. The obtained indigo fruit anthocyanin has a weight of 50.9g, wherein the purity of the anthocyanin is 21.69%.
The above embodiments are only for illustrating the technical concept and the technical features of the present invention, and the protection scope of the present invention is not limited thereby. All equivalent changes or modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (7)
1. A method for preparing indigo fruit anthocyanin from indigo fruit is characterized by comprising the following steps:
(1) crushing and pulping fresh indigo honeysuckle fruits by adopting a colloid mill to obtain fruit pulp;
(2) extracting the fruit pulp obtained in the step (1) by using a subcritical water extraction technology in the presence of an antioxidant;
(3) introducing the feed liquid extracted in the step (2) into a centrifuge for centrifugation, and collecting a centrifugate;
(4) standing the centrifugate obtained in the step (3) to room temperature for layering, collecting a lower water layer, and filtering the water layer to obtain a filtrate A;
(5) winterizing the filtrate A in the step (4), and then filtering again to obtain a filtrate B;
(6) treating the filtrate B in the step (5) by adopting a ceramic membrane and a nanofiltration membrane in sequence to obtain a concentrated solution A;
(7) concentrating the concentrated solution A in the step (6) by adopting molecular distillation to obtain a concentrated solution B;
(8) and (5) carrying out vacuum freeze drying on the concentrated solution B in the step (7) to obtain finished product powder containing the lonicera edulis anthocyanin.
2. The method for preparing indigo fruit anthocyanin from indigo fruit as claimed in claim 1, wherein the method comprises the following steps: in the step (2), the indigo fruit pulp is extracted by adopting a subcritical water extraction technology, the pressure range is 16-20 MPa, the extraction temperature is 300-340 ℃, and the fruit pulp: water =1: 1-3 (m/m), extraction time is 10-30 min, and extraction is performed for 2 times.
3. The method for preparing indigo fruit anthocyanin from indigo fruit as claimed in claim 1, wherein the method comprises the following steps: in the step (2), the added antioxidant is EGCG, and the addition amount of the 2 times of extraction is 0.01-0.05% of the weight of the lonicera edulis.
4. The method for preparing indigo fruit anthocyanin from indigo fruit as claimed in claim 1, wherein the method comprises the following steps: in the step (5), the winterization temperature is 1-5 ℃, and the winterization time is 5-10 h.
5. The method for preparing indigo fruit anthocyanin from indigo fruit as claimed in claim 1, wherein the method comprises the following steps: in the step (6), a membrane element with the aperture of 200nm is selected as the aperture of the ceramic membrane, the temperature of the ceramic membrane treatment solution is 21-25 ℃, and the pressure is 0.2-0.4 MPa; the molecular weight cut-off of the nanofiltration membrane is 200-400 Da, the temperature of the nanofiltration membrane treatment liquid is 23-28 ℃, and the pressure is 0.3-0.5 MPa.
6. The method for preparing indigo fruit anthocyanin from indigo fruit as claimed in claim 1, wherein the method comprises the following steps: in the step (7), the pressure of molecular distillation is 20-30 Pa, the evaporation temperature is 30-35 ℃, the condensation temperature is 0-10 ℃, and the material flow rate is 1.0-2.0L/min.
7. The method for preparing anthocyanin from indigo fruit as claimed in claim 1, wherein: in the step (8), the vacuum degree is controlled to be 10-13 Pa during freezing, the temperature is controlled to be-50 to-40 ℃, and the freezing and drying are carried out until the moisture content is below 5 percent.
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| CN201811110903.XA CN110938054A (en) | 2018-09-25 | 2018-09-25 | Method for preparing indigo fruit anthocyanin from indigo fruit |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110669035A (en) * | 2019-10-07 | 2020-01-10 | 大兴安岭至臻尚品寒带生物技术有限公司 | Method for preparing anthocyanin from indigo fruit |
| CN115572493A (en) * | 2022-09-23 | 2023-01-06 | 廊坊师范学院 | Method for preparing natural plant toner from fruit and vegetable raw materials |
| CN116693492A (en) * | 2023-04-17 | 2023-09-05 | 大兴安岭至臻尚品寒带生物技术有限公司 | Method for preparing lonicera caerulea anthocyanin from lonicera caerulea |
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2018
- 2018-09-25 CN CN201811110903.XA patent/CN110938054A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110669035A (en) * | 2019-10-07 | 2020-01-10 | 大兴安岭至臻尚品寒带生物技术有限公司 | Method for preparing anthocyanin from indigo fruit |
| CN115572493A (en) * | 2022-09-23 | 2023-01-06 | 廊坊师范学院 | Method for preparing natural plant toner from fruit and vegetable raw materials |
| CN116693492A (en) * | 2023-04-17 | 2023-09-05 | 大兴安岭至臻尚品寒带生物技术有限公司 | Method for preparing lonicera caerulea anthocyanin from lonicera caerulea |
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Application publication date: 20200331 |