CN-122010891-A - Aronia melanocarpa anthocyanin purification process and equipment

CN122010891ACN 122010891 ACN122010891 ACN 122010891ACN-122010891-A

Abstract

The invention discloses a purification process and equipment of aronia melanocarpa anthocyanin, wherein the process comprises the steps of preprocessing and crushing raw materials to prepare fruit powder, mixing the fruit powder with an acidic solvent, introducing inert gas for ultrasonic extraction, carrying out fractional filtration and low-temperature concentration on an extract to obtain a crude concentrated solution, regulating and controlling magnetic macroporous adsorption resin to form a uniform bed layer through a gradient magnetic field, carrying out chromatographic adsorption on the concentrated solution, and carrying out gradient elution, secondary concentration, biphase extraction, drying and stabilizing treatment to obtain a finished product. The invention improves the anthocyanin adsorption efficiency and separation precision by means of magnetic resin and gradient magnetic control design, improves the purity and activity retention rate of the product, and meets the requirement of large-scale production.

Inventors

JI CHUNHE
ZHANG JINGHONG
CAI ZHIHUI
YANG ZHEN

Assignees

秦皇岛市禾采农业科技开发有限公司

Dates

Publication Date: 20260512
Application Date: 20251217

Claims (10)

1. The process for purifying the anthocyanin of the aronia melanocarpa is characterized by comprising the following steps of: s100, raw material pretreatment and crushing, namely sequentially screening, cleaning, crushing, degreasing, drying and crushing the raw materials of the aronia melanocarpa to obtain aronia melanocarpa fruit powder; S200, extracting, namely mixing the aronia melanocarpa fruit powder with an acidic extraction solvent, introducing inert gas to form a protective atmosphere, and performing ultrasonic auxiliary extraction to obtain an extracting solution; s300, carrying out graded filtration, namely sequentially carrying out rough filtration and fine filtration on the extracting solution, removing solid impurities and macromolecular colloids, and collecting a permeate; s400, concentrating at low temperature, namely concentrating the permeate at low temperature to obtain crude concentrate; S500, magnetic field regulation chromatography purification, namely preparing magnetic macroporous adsorption resin, filling the magnetic macroporous adsorption resin between two support sieve plates in a chromatographic column, generating a gradient magnetic field gradually increasing along the flow direction of feed liquid through a magnetic field regulation device, driving the magnetic macroporous adsorption resin particles to locally finely adjust the positions to form a uniform stationary phase bed layer, and introducing the crude extract concentrate into the chromatographic column according to the gradient flow velocity gradually decreasing along the flow direction of the feed liquid to finish anthocyanin adsorption; s600, gradient elution, namely sequentially adopting deionized water, low-concentration ethanol solution and high-concentration ethanol solution to perform gradient elution on the chromatographic column, and collecting anthocyanin enrichment eluent; and S700, refining, namely sequentially carrying out secondary concentration, biphase extraction impurity removal, drying forming and stabilization treatment on the anthocyanin enrichment eluent to obtain the finished product of the aronia melanocarpa anthocyanin.
2. The process for purifying an aronia according to claim 1, wherein in step S500, the magnetic macroporous adsorption resin is prepared by the following steps: s510, preprocessing a matrix, namely taking macroporous adsorption resin, soaking and activating the macroporous adsorption resin by using ethanol with the volume fraction of 95%, washing the macroporous adsorption resin to be neutral by using deionized water, and drying the macroporous adsorption resin in vacuum; S520, carrying out in-situ loading on the magnetic cores, namely dispersing the pretreated macroporous adsorption resin in deionized water to form a suspension, adding a mixed solution of ferrous sulfate and ferric chloride, wherein the molar ratio of ferrous ions to ferric ions is 1:2, dropwise adding ammonia water to adjust the pH value to be alkaline, and then heating and preserving heat to enable the ferroferric oxide cores to be deposited on the surface and in pores of the resin in situ; s530, coating an isolation layer, namely adding a silane coupling agent into the suspension, and heating to react to form a silicon dioxide isolation layer on the surface of the ferroferric oxide core; S540, post-treatment, namely separating the resin, washing the resin to be neutral, and drying the resin to obtain the magnetic macroporous adsorption resin.
3. The process for purifying the aronia melanocarpa anthocyanin according to claim 2, wherein in the step S520, the total mass of the mixed solution is 15% -25% of the mass of the macroporous adsorbent resin, and in the step S530, the silane coupling agent is 3% -8% of the mass of the macroporous adsorbent resin, and the silane coupling agent is added after being diluted by ethanol in advance.
4. The process for purifying the anthocyanin in the aronia melanocarpa according to claim 1, wherein in the step S500, the gradient magnetic field is formed by two sections of independent magnetic field generating units which are axially arranged along the chromatographic column, and the gradient flow rate and the magnetic field intensity gradient are reversely adapted to realize the sufficient adsorption of the anthocyanin with different molecular weights.
5. The process for purifying the anthocyanin from the aronia melanocarpa according to claim 1, wherein in the step S600, the volume fraction of the low-concentration ethanol solution is 15% -25%, the volume fraction of the high-concentration ethanol solution is 65% -75%, and the elution flow rates of the deionized water, the low-concentration ethanol solution and the high-concentration ethanol solution are sequentially decreased in the elution process.
6. The purification equipment for the aronia melanocarpa anthocyanin is used for realizing the purification process of any one of claims 1-5 and is characterized by comprising a magnetic control chromatography device, a raw material treatment device, an ultrasonic material lifting device, a grading filter material device, a low-temperature concentration device, a gradient leaching device and a refined material receiving device which are sequentially in flange butt joint with the magnetic control chromatography device through a sealing conveying pipeline, wherein the shell of each device is made of an anti-corrosion metal material, a sealing gasket is arranged at the interface of the sealing conveying pipeline and each device, and the purification equipment further comprises an integrated control box which is electrically connected with an execution part of each device through a cable, wherein a closed cavity for filling magnetic macroporous adsorption resin is formed inside the magnetic control chromatography device.
7. The device for purifying the anthocyanin of the aronia melanocarpa according to claim 6, wherein the magnetic control chromatography device comprises a chromatography column casing (1), an upper sieve plate assembly (2) and a lower sieve plate assembly (3), the chromatography column casing (1) is a hollow cylinder with flanges at two ends, the upper sieve plate assembly (2) comprises an upper sieve plate body (20) which is a porous plate structure, is fixedly connected with the inner wall of the chromatography column casing (1) and is detachably arranged, the lower sieve plate assembly (3) comprises a fixed sieve plate (30), a movable sieve plate (31) and lifting support rods (32), the fixed sieve plate (30) is arranged in the middle of the chromatography column casing (1) and forms a leakage gap (33) with the inner wall of the chromatography column casing (1), the movable sieve plate (31) is slidably arranged in the chromatography column casing (1) and is connected with lifting support rods (32), and the movable sieve plate (31) and the fixed sieve plate (30) can be spliced to seal the leakage gap (33).
8. The device for purifying the anthocyanin of the aronia melanocarpa according to claim 7, wherein the magnetic control chromatography device further comprises a gradient magnetic control assembly (4), the gradient magnetic control assembly (4) comprises at least two sections of magnetic coil units, each magnetic coil unit comprises an insulating framework (40), an enamelling coil (41) and a wiring terminal, the insulating framework (40) is of a cylindrical structure sleeved on the outer wall of the chromatography column casing (1), the enamelling coil (41) is wound on the outer side of the insulating framework (40), the wiring terminal is fixedly arranged at the end of the insulating framework (40) and is electrically connected with the enamelling coil (41), the number of turns of the enamelling coil (41) of each magnetic coil unit is sequentially increased from a feeding end to a discharging end along the axial direction of the chromatography column casing (1), and the outer side of each magnetic coil unit is coated with a magnetic shielding cover (42).
9. The device for purifying the anthocyanin of the aronia melanocarpa according to claim 7, wherein the magnetic control chromatography device further comprises a temperature control assembly (5) and a discharge hopper (6), the temperature control assembly (5) comprises a spiral heat exchange tube (50) fixed in the chromatography column casing (1), a water inlet and a water outlet of the spiral heat exchange tube are respectively arranged at the lower part and the upper part of two sides, the device further comprises a temperature measurement probe (51) arranged in the chromatography column casing (1), the discharge hopper (6) is of a conical structure, the large-caliber end of the discharge hopper is in sealing butt joint with the flange at the bottom end of the chromatography column casing (1), the small-caliber end of the discharge hopper is provided with a discharge tube (8) with a pneumatic valve (7), and the discharge tube (8) is in flange connection with a sealing and conveying pipeline of the refining receiving device.
10. The device for purifying the anthocyanin of the aronia melanocarpa according to claim 8, wherein the magnetic control chromatography device further comprises a gas-assisted discharge assembly, the gas-assisted discharge assembly comprises a gas flow connecting pipe (9) and a regulating valve group, one end of the gas flow connecting pipe (9) is obliquely connected to the side wall of the discharge hopper (6) and is communicated with the inside of the discharge hopper (6), the other end of the gas flow connecting pipe is connected with a high-pressure gas source through a quick-plug connector, the regulating valve group comprises an electromagnetic stop valve and a flow regulating valve, the electromagnetic stop valve and the flow regulating valve are connected to the gas flow connecting pipe (9) in series, the electromagnetic stop valve is electrically connected with an integrated control box through a cable, and the lower end of the lifting support rod (32) is connected with a driving cylinder (34), and the driving cylinder (34) and the electromagnetic stop valve are in linkage control through the integrated control box.

Description

Aronia melanocarpa anthocyanin purification process and equipment Technical Field The invention relates to the technical field of anthocyanin purification, in particular to an aronia melanocarpa anthocyanin purification process and equipment. Background The aronia melanocarpa is rich in polyphenol active ingredients such as anthocyanin, and the purification process of the aronia melanocarpa becomes a research hot spot in the field of foods and health products. The main purification technology in the industry at present is a macroporous adsorption resin fixed bed process, and the process realizes the separation of anthocyanin and impurities through the flow of raw material pretreatment, ultrasonic extraction, membrane filtration, fixed bed resin adsorption, gradient elution, concentration and drying, and is widely applied to industrial production due to the advantages of simple operation, controllable cost, easy scale and the like. The macroporous adsorption resin is used as a core purification medium by virtue of high adsorption selectivity on anthocyanin, and an adsorption mechanism of the macroporous adsorption resin mainly depends on the hydrophobic effect, van der Waals force and hydrogen bonding effect of resin pores to realize anthocyanin enrichment and impurity removal. However, in the prior art, resin particles are filled in a column body by a fixed bed resin column by means of gravity, and in the natural sedimentation process of the resin particles, local compact areas and gaps are easy to form, wherein the resin in the compact areas is closely accumulated, the flowing resistance of feed liquid is high, and the resistance of the gap areas is low, so that the feed liquid flows fast along the gaps preferentially to form 'channeling'. The phenomenon causes that part of resin cannot fully contact with feed liquid to form an adsorption 'dead zone', a large number of adsorption sites are wasted, anthocyanin in a 'channeling' area is not fully adsorbed due to insufficient contact time with the resin, namely leakage along with effluent liquid, and the problem of 'penetration advance' occurs. Disclosure of Invention The invention mainly aims to provide an aronia melanocarpa anthocyanin purification process and equipment, which realize high-efficiency adsorption and accurate separation of anthocyanin by customizing magnetic adsorption resin, gradient magnetic control chromatography design and special equipment structure innovation, improve the purity and activity retention rate of the product, simplify the resin recovery process, enhance the operation stability of equipment and meet the requirement of large-scale production. In order to achieve the above purpose, the invention provides an aronia melanocarpa anthocyanin purification process, which comprises the following steps: s100, raw material pretreatment and crushing, namely sequentially screening, cleaning, crushing, degreasing, drying and crushing the raw materials of the aronia melanocarpa to obtain aronia melanocarpa fruit powder; S200, extracting, namely mixing the aronia melanocarpa fruit powder with an acidic extraction solvent, introducing inert gas to form a protective atmosphere, and performing ultrasonic auxiliary extraction to obtain an extracting solution; s300, carrying out graded filtration, namely sequentially carrying out rough filtration and fine filtration on the extracting solution, removing solid impurities and macromolecular colloids, and collecting a permeate; s400, concentrating at low temperature, namely concentrating the permeate at low temperature to obtain crude concentrate; S500, magnetic field regulation chromatography purification, namely preparing magnetic macroporous adsorption resin, filling the magnetic macroporous adsorption resin between two support sieve plates in a chromatographic column, generating a gradient magnetic field gradually increasing along the flow direction of feed liquid through a magnetic field regulation device, driving the magnetic macroporous adsorption resin particles to locally finely adjust the positions to form a uniform stationary phase bed layer, and introducing the crude extract concentrate into the chromatographic column according to the gradient flow velocity gradually decreasing along the flow direction of the feed liquid to finish anthocyanin adsorption; s600, gradient elution, namely sequentially adopting deionized water, low-concentration ethanol solution and high-concentration ethanol solution to perform gradient elution on the chromatographic column, and collecting anthocyanin enrichment eluent; and S700, refining, namely sequentially carrying out secondary concentration, biphase extraction impurity removal, drying forming and stabilization treatment on the anthocyanin enrichment eluent to obtain the finished product of the aronia melanocarpa anthocyanin. In one possible embodiment, in step S500, the preparation steps of the magnetic macroporous adsorbent resin are as follows: s510,