Method and system for efficiently extracting blueberry anthocyanin

Abstract

The invention relates to a method for efficiently extracting blueberry anthocyanin and an extraction system.The method for efficiently extracting the blueberry anthocyanin comprises the steps that blueberries are squeezed through a belt type squeezer, and the squeezed blueberries are divided into blueberry juice and blueberry pomace; adding water of which the weight is 5-10 times that of the blueberry residues into the blueberry residues, mixing, and adjusting the pH value; carrying out enzymolysis by adopting a compound enzyme; during enzymolysis, filtering by using a duplex filter, extracting into an adsorption tank, adsorbing enzymatic hydrolysate by using macroporous resin, after anthocyanin in the enzymatic hydrolysate is adsorbed, filtering, injecting into the enzymolysis tank, performing enzymolysis again, and performing circular treatment; after the elution is finished, filtering the eluent through a baffle plate, carrying out vacuum concentration, removing ethanol, and carrying out secondary separation and purification on the eluent by using polyamide resin; carrying out vacuum concentration on the eluent again, and completely removing ethanol; according to the method, the material cost of blueberry anthocyanin extraction is reduced, the extraction period is shortened, and the production efficiency is improved.

Description

Technical Field

[0001] The present invention belongs to the technical field of deep processing of blueberries, and specifically relates to a method and an extraction system for efficiently extracting blueberry anthocyanins. Background Art

[0002] Blueberries are perennial shrubs with small berries and are rich in nutrients. They are recommended by the Food and Agriculture Organization of the World as "the world's third-generation fruits". Anthocyanins in blueberries are their main bioactive substances and have various physiological and active functions such as preventing brain nerve aging, protecting eyesight, strengthening the heart, anti-cancer, softening blood vessels, and enhancing the body's immune function. In March 2023, the National Health Commission approved blueberry anthocyanins as a new food raw material, which can be used in a variety of food and beverages. This provides strong legal protection for the commercialization of blueberry extracts and will greatly promote the development of the blueberry deep processing industry.

[0003] There are several major problems in current blueberry extraction:

[0004] 1. The extraction cost is relatively high. Most of the existing blueberry extraction technologies use blueberries as raw materials for extraction without comprehensively considering the blueberry extraction and processing, resulting in a relatively high cost of blueberry extracts. Through literature research, the main existence of blueberry anthocyanins is in the blueberry skin. Therefore, the deep processing of blueberries can be comprehensively considered. By pressing, the fruit juice in the blueberries can be mechanically separated from the pulp and skin. The blueberry juice can be used to produce fruit juice beverages, and the blueberry pulp and skin can be used for the extraction of blueberry anthocyanins. The advantage of this is that it can not only reduce the cost of blueberry extracts but also separate the water and carbohydrates in the blueberries through pressing, reducing the subsequent separation steps for blueberry anthocyanin extraction and improving the extraction efficiency.

[0005] 2. The extraction process cycle is relatively long. Currently, most blueberry extraction processes add extraction solutions according to about 10 times the blueberry material, and then carry out enzymatic hydrolysis, extraction, filtration, separation and purification, concentration, freeze-drying or spray-drying. Each process can only enter the next process after it is completed, and the separation and purification takes a long time. Once the effect is not ideal, secondary separation and purification are required, which is time-consuming and laborious. Improving the blueberry extraction efficiency and quality and shortening the extraction cycle have high economic value and practical significance. Summary of the Invention

[0006] The purpose of this part is to outline some aspects of the embodiments of the present invention and briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this part, as well as in the abstract and title of the present application, to avoid obscuring the purpose of this part, the abstract, and the title. However, such simplifications or omissions cannot be used to limit the scope of the present invention.

[0007] In view of the following technical problems existing in the prior art:

[0008] 1. The cost of blueberry extraction is high, the blueberries are not pretreated, and the deep processing of blueberries is not comprehensively considered.

[0009] 2. The blueberry extraction cycle is relatively long. The traditional technology is to carry out each extraction process in sequence, among which separation and purification are the key links that affect the extraction cycle, resulting in low efficiency of the entire extraction process.

[0010] In order to solve the above technical problems, the present invention provides the following technical solutions: a method for efficiently extracting anthocyanins from blueberry, comprising:

[0011] Blueberries are squeezed with a belt press and separated into blueberry juice and blueberry pomace. Blueberry juice can be used to produce blueberry juice drinks. After squeezing, the quality of blueberries will be reduced to 20%-30% of the original.

[0012] Add 5-10 times the weight ratio of water to the blueberry residue and mix, and adjust the pH of the solution to 2.8-4.0 with citric acid, sodium citrate and phosphoric acid;

[0013] Using compound enzyme for enzymatic hydrolysis;

[0014] During enzymatic hydrolysis, the solution is filtered through a double filter and then extracted into an adsorption tank. The enzymatic hydrolyzate is adsorbed by a macroporous resin. After anthocyanins in the enzymatic hydrolyzate are adsorbed, the solution is filtered and then injected into the enzymatic hydrolysis tank for further enzymatic hydrolysis, and the treatment is circulated;

[0015] After the enzymatic hydrolysis-adsorption is completed, a 50-70% ethanol solution is injected into the adsorption tank for stirring and elution. After the elution is completed, the eluate is filtered through a baffle and then concentrated by vacuum to remove most of the ethanol in the eluate, so that the concentration of the eluate is less than 20%;

[0016] The eluate is separated and purified for a second time using a polyamide resin;

[0017] The eluate was concentrated again under reduced pressure to completely remove ethanol.

[0018] As a preferred technical solution for a method for efficiently extracting anthocyanins from blueberry, the complex enzyme comprises: 2-3 parts of cellulase, 1-2 parts of pectinase, and 0-1 part of hemicellulase; the complex enzyme is added at 0.1-2.0% of the total weight; the enzymatic hydrolysis conditions are: stirring speed 10-30rpm / min; enzymatic hydrolysis temperature 30-50°C; and enzymatic hydrolysis time: 40-60min.

[0019] As a preferred technical solution for a method for efficiently extracting anthocyanins from blueberry, the secondary separation and purification parameters include: sample loading speed 0.5-2.0 BV / h; ethanol solution concentration 60-75%; ethanol solution flow rate 0.5-2.0 BV / h; and ethanol solution dosage 1.5-3.0 times column volume.

[0020] The present invention also discloses an extraction system based on the aforementioned method for efficiently extracting blueberry anthocyanins, which includes an enzymatic hydrolysis tank, an adsorption tank, and a vacuum concentration tank. A first discharge pipe is provided at the bottom of the enzymatic hydrolysis tank, and a screw pump and a double-filter are arranged on the first discharge pipe. A first feed pipe is provided at the top of the enzymatic hydrolysis tank.

[0021] As a preferred technical solution of an extraction system for efficiently extracting blueberry anthocyanins, a second feed pipe is provided at the top of the adsorption tank. The first discharge pipe is connected to the second feed pipe through a first valve. A third feed pipe is further included, and the third feed pipe is connected to the second feed pipe through a first valve. A first observation port is arranged on the second feed pipe.

[0022] As a preferred technical solution of an extraction system for efficiently extracting blueberry anthocyanins, a second discharge pipe is provided at the bottom of the adsorption tank. A centrifugal pump is arranged on the second discharge pipe. The second discharge pipe is communicated with the first feed pipe through a second valve. A second observation port is arranged on the second discharge pipe.

[0023] As a preferred technical solution of an extraction system for efficiently extracting blueberry anthocyanins, a fourth discharge pipe is provided at the top of the vacuum concentration tank, and a third discharge pipe is provided at the bottom. A fourth feed pipe is arranged on the side of the vacuum concentration tank, and the fourth feed pipe is connected to the second valve.

[0024] As a preferred technical solution of an extraction system for efficiently extracting blueberry anthocyanins, a first stirring blade is arranged in the enzymatic hydrolysis tank, and a first filter plate is further arranged near the bottom of the enzymatic hydrolysis tank. A first stirring blade is arranged in the adsorption tank, and a second filter plate is arranged near the bottom of the adsorption tank. A nozzle is further arranged at the end of the second feed pipe.

[0025] As a preferred technical solution of an extraction system for efficiently extracting blueberry anthocyanins, the double-filter includes a first branch and a second branch arranged in parallel. A first filter tube is arranged on the first branch, and a second filter tube is arranged on the second branch.

[0026] The beneficial effects of the present invention:

[0027] 1. Reduce the material cost of blueberry anthocyanin extraction. Considering the whole process of blueberry deep processing, using the by-product fruit residue after blueberry juice extraction as the raw material for blueberry anthocyanin extraction can greatly reduce the material cost of blueberry anthocyanin extraction. At the same time, the by-product blueberry residue can be fully reused, which can greatly improve the overall economic value of blueberry deep processing.

[0028] 2. Shorten the extraction cycle. The patent creatively combines the enzymatic hydrolysis process in the extraction process with the first separation and purification process. Through filtration circulation, the enzymatic hydrolysate is circulated to the adsorption tank, and the macroporous resin is used to adsorb the anthocyanins released in the enzymatic hydrolysate. This can reduce the time of the entire anthocyanin extraction, separation and purification process and greatly improve the efficiency of anthocyanin extraction and separation. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following will briefly introduce the drawings required for the description of the embodiments. Obviously, the drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings. Among them:

[0030] Figure 1 It is a schematic structural diagram of the method flow of the present invention;

[0031] Figure 2 It is a schematic overall structure diagram of the extraction system in the present invention;

[0032] Figure 3 It is a schematic cross-sectional structure diagram of the extraction system in the present invention;

[0033] Figure 4 It is a schematic diagram of the frame connection structure of the extraction system in the present invention.

[0034] Reference numerals: 102, screw pump; 101, first discharge pipe; 203, third feed pipe; 202, first valve; 201a, first observation port; 205, centrifugal pump; 104, first feed pipe; 204, second discharge pipe; 204a, second observation port; 301, fourth discharge pipe; 302, third discharge pipe; 300, vacuum concentration tank; 303, fourth feed pipe; 206, second valve; 105, first stirring blade; 100, enzymatic hydrolysis tank; 106, first filter plate; 207, second stirring blade; 200, adsorption tank; 208, second filter plate; 201, second feed pipe; 209, spray head; 103, double filter; 400, first branch; 401, first filter pipe; 500, second branch; 501, second filter pipe. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0035] In order to make the above objects, features and advantages of the present invention more obvious and understandable, the following will make a detailed description of the specific embodiments of the present invention with reference to the accompanying drawings of the specification.

[0036] In the following description, many specific details are set forth to facilitate a full understanding of the present invention, but the present invention may also be implemented in other ways different from those described herein, and those skilled in the art may make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0037] Secondly, the term "one embodiment" or "embodiment" as used herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The term "in one embodiment" that appears in different places in this specification does not necessarily refer to the same embodiment, nor does it refer to a separate or selective embodiment that is mutually exclusive with other embodiments.

[0038] Secondly, the present invention is described in detail with reference to the schematic diagram. When describing the embodiments of the present invention in detail, for the sake of convenience, the cross-sectional diagrams showing the device structure will not be partially enlarged according to the general scale, and the schematic diagrams are only examples, which should not limit the scope of protection of the present invention. In addition, in actual production, the three-dimensional dimensions of length, width and depth should be included.

[0039] Example 1

[0040] Reference Figures 1 to 4 This embodiment provides a method for efficiently extracting blueberry anthocyanins.

[0041] The steps include:

[0042] 1. Belt pressing: fresh blueberries / blueberry frozen fruits (thawed at room temperature) are squeezed with a belt press to obtain blueberry juice and blueberry pomace respectively;

[0043] 2. Add 5-10 times the weight ratio of water to the blueberry residue and mix them. Adjust the pH of the solution to 2.8-4.0 with citric acid, sodium citrate and phosphoric acid.

[0044] 3. Use cellulase, pectinase and hemicellulase for enzymolysis. The compound ratio of the three enzymes is: 2-3 parts of cellulase, 1-2 parts of pectinase, and 0-1 part of hemicellulase; the compound enzyme is added at 0.1-2.0% of the total weight; enzymolysis conditions: stirring speed 10-30rpm / min; enzymolysis temperature 30-50℃; enzymolysis time: 40-60min;

[0045] 4. After a period of enzymatic hydrolysis, the anthocyanins in the enzymatic hydrolysate are roughly adsorbed by macroporous resin; the enzymatic hydrolysate in the enzymatic hydrolysate tank is pumped into a double filter with a screw pump for 200 mesh filtration and then pumped into an adsorption tank. There is a spray device on the top of the adsorption tank to evenly spray the enzymatic hydrolysate on the macroporous resin. The macroporous resin model used is one of AB-8, D101, and XDA-7HP;

[0046] There is a 80-mesh baffle at the bottom of the enzymatic hydrolysis tank to ensure that materials with larger particles do not enter the double filter, thus improving the filtration efficiency.

[0047] Double filter: Once there is a lot of filter residue in the filter, another filter is used to remove the filter residue to ensure the continuous progress of the entire extraction process. There is a 400-mesh filter bag in the double filter.

[0048] There is a paddle-type stirring device in the adsorption tank. When adsorption starts, the stirring is turned on, and the stirring speed is 5 - 10 rpm / min. The resin is in an up-and-down tumbling state under stirring. There is a 100-mesh filtering device at the bottom of the adsorption tank. The filtrate after adsorption is filtered and pumped to the top of the enzymatic hydrolysis tank by a centrifugal pump, and the filtrate is added to the enzymatic hydrolysate. In this way, a dynamic cycle is formed between the enzymatic hydrolysis tank and the adsorption tank, and a system for continuous enzymatic hydrolysis and adsorption is established.

[0049] 5. The solution in the observation port B should be light pink or colorless. If the color becomes darker, an appropriate amount of macroporous resin can be added to the adsorption tank.

[0050] 6. When the color of the solution in the observation port A becomes light pink or colorless, it is preliminarily determined that the extraction is completed.

[0051] 7. After the extraction and adsorption are completed, an ethanol solution with a concentration of 50 - 70% is pumped into the adsorption tank. The ethanol solution is sprayed onto the macroporous resin through the spray head of the adsorption tank. The paddle stirring in the adsorption tank is turned on simultaneously, and the stirring speed is 5 - 10 rpm / min. The solution eluted at the bottom is pumped to the storage tank by pump B. Until the color of the macroporous resin in the adsorption tank becomes light white or colorless, and at the same time, the solution in the observation port B is transparent or colorless. The elution is completed.

[0052] 8. The eluate of the macroporous resin is vacuum concentrated to remove ethanol. The concentration temperature is 30 - 50 °C, and finally the ethanol in the eluate of the macroporous resin is concentrated to about 10 - 20%.

[0053] 9. The elution solution is further separated and purified with polyamide resin. Loading condition parameters: loading speed 0.5 - 2.0 BV / h; elution condition parameters: ethanol solution concentration 60 - 75%; ethanol solution flow rate 0.3 - 1.5 BV / h; ethanol solution dosage 1.5 - 3.0 times the column volume.

[0054] 10. The eluate is concentrated under reduced pressure. The concentration temperature is 30 - 50 °C, and ethanol is evaporated from the eluate.

[0055] 11. The concentrated eluate is freeze-dried.

[0056] This embodiment also provides an extraction system based on the aforementioned method for efficiently extracting blueberry anthocyanins, including an enzymolysis tank 100, an adsorption tank 200, and a vacuum concentration tank 300. A first discharge pipe 101 is provided at the bottom of the enzymolysis tank 100, and a screw pump 102 and a double filter 103 are arranged on the first discharge pipe 101. A first feed pipe 104 is provided at the top of the enzymolysis tank 100.

[0057] A second feed pipe 201 is provided at the top of the adsorption tank 200. The first discharge pipe 101 is connected to the second feed pipe 201 through a first valve 202. It further includes a third feed pipe 203, and the third feed pipe 203 is connected to the second feed pipe 201 through the first valve 202. A first observation port 201a is arranged on the second feed pipe 201.

[0058] A second discharge pipe 204 is provided at the bottom of the adsorption tank 200, and a centrifugal pump 205 is arranged on the second discharge pipe 204. The second discharge pipe 204 is communicated with the first feed pipe 104 through a second valve 206. A second observation port 204a is arranged on the second discharge pipe 204.

[0059] A fourth discharge pipe 301 is provided at the top of the vacuum concentration tank 300, and a third discharge pipe 302 is provided at the bottom. A fourth feed pipe 303 is arranged on the side of the vacuum concentration tank 300, and the fourth feed pipe 303 is connected to the second valve 206.

[0060] It should be noted that the second valve 206 is a three-way valve with one inlet and two outlets. The inlet is connected to the second discharge pipe 204, and the two outlets are connected to the fourth feed pipe 303 and the first feed pipe 104. The first valve 202 is a three-way valve with two inlets and one outlet. The two inlets are connected to the third feed pipe 203 and the first discharge pipe 101, and the outlet is connected to the second feed pipe 201. An ethanol solution of 50%-70% can be added to the adsorption tank 200 from the third feed pipe 203.

[0061] When the second discharge pipe 204 is connected to the first feed pipe 104, and the second feed pipe 201 is connected to the first discharge pipe 101, the solution is dynamically circulated between the enzymolysis tank 100 and the adsorption tank 200 to fully enzymolyze and adsorb and extract the solution. When the adsorption reaches a certain level, that is, when the filtrate transported from the adsorption tank 200 to the enzymolysis tank 100 is observed to be light red or colorless from the second observation port 204a, it can be determined that the adsorption and extraction is sufficient, the solution in the adsorption tank 200 is emptied, and the second valve 206, the centrifugal pump 205 and the spiral are closed. Pump 102 connects the first valve 202 to the second feed pipe 201 and the third feed pipe 203, adds 50%-70% ethanol solution to the adsorption tank 200 and stirs it thoroughly to dissolve the components to be extracted into the ethanol solution, then connects the second discharge pipe 204 and the fourth feed pipe 303, injects the ethanol solution into the vacuum concentration tank 300, and the ethanol evaporates and leaves from the fourth discharge pipe 301. The eluent containing 10%-20% ethanol is discharged from the third discharge pipe 302 and is used for secondary separation and purification with polyamide resin.

[0062] The enzymolysis tank 100 is provided with a first stirring blade 105, and a first filter plate 106 is also provided near the bottom of the enzymolysis tank 100. The adsorption tank 200 is provided with a first stirring blade 207, and a second filter plate 208 is provided near the bottom of the adsorption tank 200. A nozzle 209 is also provided at the end of the second feed pipe 201.

[0063] The first filter plate 106 has an 80-mesh size, and the second filter plate 208 has a 100-mesh size.

[0064] The duplex filter 103 includes a first branch 400 and a second branch 500 which are arranged in parallel. The first branch 400 is provided with a first filter tube 401 , and the second branch 500 is provided with a second filter tube 501 .

[0065] It should be noted that both ends of the duplex filter 103 are connected to the first discharge pipe 101 through three-way valves.

[0066] The efficiency of the present invention is verified by comparing the time consumed by different extraction processes.

[0067] Taking the extraction of 5kg of blueberry residue as an example, the traditional and patented extraction and separation processes (involving only the front-end enzyme desorption adsorption and elution process, not the subsequent acetamide separation and purification) were used respectively. After comparison, the relevant data are as follows:

[0068] Comparison of time consumption of different extraction processes

[0069]

[0070] It should be understood that, during the development of any actual implementation, such as in any engineering or design project, numerous specific implementation decisions can be made. Such development efforts may be complex and time-consuming, but for those of ordinary skill in the art who benefit from this disclosure, without undue experimentation, such development efforts will be routine work in design, manufacturing, and production.

[0071] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the spirit and scope of the technical solutions of the present invention, and they should all be covered within the scope of the claims of the present invention.

Claims

1. A method for efficiently extracting blueberry anthocyanins, characterized in that: include, The blueberries are squeezed and separated into blueberry juice and blueberry pomace after squeezing; Add 5-10 times the amount of water to the blueberry residue and mix, and adjust the pH of the solution to 2.8-4.0 with citric acid, sodium citrate, and phosphoric acid; Using compound enzyme for enzymatic hydrolysis; During enzymatic hydrolysis, the enzymatic hydrolysate is filtered through a double filter and then extracted into an adsorption tank. The macroporous resin in the adsorption tank adsorbs anthocyanins in the enzymatic hydrolysate and then, after filtration, is injected into the enzymatic hydrolysis tank for further enzymatic hydrolysis, and the treatment is circulated; After the enzymatic hydrolysis-adsorption is completed, a 50-70% ethanol solution is injected into the adsorption tank for stirring and elution. After the elution is completed, the eluate is filtered through a baffle and then concentrated by vacuum to remove most of the ethanol in the eluate, so that the ethanol concentration of the eluate is less than 20%; The eluate is separated and purified for a second time using a polyamide resin; The eluate was concentrated again in vacuo to completely remove ethanol.

2. The method for efficiently extracting blueberry anthocyanins according to claim 1, characterized in that: The complex enzyme comprises: 2-3 parts of cellulase, 1-2 parts of pectinase, and 0-1 parts of hemicellulase; the complex enzyme is added at 0.1-2.0% of the total weight; the enzymolysis conditions are: stirring speed 10-30rpm / min; enzymolysis temperature 30-50℃; enzymolysis time: 40-60min.

3. The method for efficiently extracting blueberry anthocyanins according to claim 2, characterized in that: The secondary separation and purification parameters include: sample loading speed 0.5-2.0 BV / h; ethanol solution concentration 60-75%; ethanol solution flow rate 0.5-2.0 BV / h; ethanol solution dosage 1.5-3.0 times column volume.

4. An extraction system for the method of efficiently extracting blueberry anthocyanins according to any one of claims 1 to 3, characterized in that: The invention comprises an enzymolysis tank (100), an adsorption tank (200) and a vacuum concentration tank (300), wherein a first discharge pipe (101) is arranged at the bottom of the enzymolysis tank (100), a screw pump (102) and a double filter (103) are arranged on the first discharge pipe (101), and a first feed pipe (104) is arranged at the top of the enzymolysis tank (100).

5. The extraction system for efficiently extracting blueberry anthocyanins according to claim 4, characterized in that: The adsorption tank (200) is provided with a second feed pipe (201) at the top, the first discharge pipe (101) is connected to the second feed pipe (201) via a first valve (202), and also includes a third feed pipe (203), the third feed pipe (203) is connected to the second feed pipe (201) via the first valve (202), and the second feed pipe (201) is provided with a first observation port (201a).

6. The extraction system for efficiently extracting blueberry anthocyanins according to claim 5, characterized in that: A second discharge pipe (204) is provided at the bottom of the adsorption tank (200), a centrifugal pump (205) is provided on the second discharge pipe (204), the second discharge pipe (204) is connected to the first feed pipe (104) via a second valve (206), and a second observation port (204a) is provided on the second discharge pipe (204).

7. The extraction system for efficiently extracting blueberry anthocyanins according to claim 6, characterized in that: The vacuum concentrator (300) is provided with a fourth discharge pipe (301) at the top and a third discharge pipe (302) at the bottom. The vacuum concentrator (300) is provided with a fourth feed pipe (303) at the side. The fourth feed pipe (303) is connected to the second valve (206).

8. The extraction system for efficiently extracting blueberry anthocyanins according to claim 7, wherein: A first stirring blade (105) is arranged in the enzymolysis tank (100), and a first filter plate (106) is further arranged near the bottom of the enzymolysis tank (100). A second stirring blade (207) is arranged in the adsorption tank (200), a second filter plate (208) is arranged near the bottom of the adsorption tank (200), and a spray head (209) is further arranged at the end of the second feed pipe (201).

9. The extraction system for efficiently extracting blueberry anthocyanins according to claim 8, characterized in that: The double - filter (103) includes a first branch (400) and a second branch (500) arranged in parallel. A first filter tube (401) is arranged on the first branch (400), and a second filter tube (501) is arranged on the second branch (500).

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