CN113397169A - Method for continuously extracting and separating multiple natural active ingredients from mulberries - Google Patents

Method for continuously extracting and separating multiple natural active ingredients from mulberries Download PDF

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Publication number
CN113397169A
CN113397169A CN202110732680.6A CN202110732680A CN113397169A CN 113397169 A CN113397169 A CN 113397169A CN 202110732680 A CN202110732680 A CN 202110732680A CN 113397169 A CN113397169 A CN 113397169A
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mulberry
exchange resin
resin column
column
cation exchange
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李伟
黄华学
贺进军
黄�俊
宋谷良
江小龙
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Hunan Huacheng Biotech Inc
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Hunan Huacheng Biotech Inc
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/02Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation containing fruit or vegetable juices
    • A23L2/04Extraction of juices
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/70Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
    • A23L2/80Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by adsorption
    • 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
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07GCOMPOUNDS OF UNKNOWN CONSTITUTION
    • C07G99/00Subject matter not provided for in other groups of this subclass
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Health & Medical Sciences (AREA)
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  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
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  • Mycology (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The method for continuously extracting and separating various natural active ingredients from the mulberries comprises the following steps: (1) crushing raw materials and leaching with cold water; (2) centrifuging; (3) adsorbing by macroporous adsorption resin; (4) and (3) separating anthocyanin: eluting with low alcohol; (5) and (3) separation of polyphenol: eluting with high ethanol; (6) desalting and decoloring: passing through a series of cation-anion exchange resin columns; (7) separation of total amino acids: eluting the cation exchange resin column with dilute ammonia water. The method can realize the comprehensive utilization of mulberry resources, and has the advantages of high product yield, high active ingredient content, simple process, strong operability, low equipment requirement, low production cost, safety, greenness, environmental protection and suitability for industrial production.

Description

Method for continuously extracting and separating multiple natural active ingredients from mulberries
Technical Field
The invention relates to a method for extracting and separating natural active ingredients of mulberries, in particular to a method for continuously extracting and separating various natural active ingredients from mulberries.
Background
Mulberries, also known as jujubes, mulberries, mulberry seeds, mulberries and the like, are polymeric succulent berries born by perennial woody plants, are cylindrical, have a length of 1-2cm and a diameter of 0.5-0.8cm, and are ripe in about 4-6 months per year. The ripe mulberry fruit is mellow, sour and sweet, and is preferably large, thick in flesh, purplish red in color and rich in sugar. The mulberry juice is thick and honey-like, sweet and sour, fragrant and rich in nutrient components, is listed as one of 'medicinal and edible' agricultural products which are both food and medicines by the national ministry of health, and is praised as 'third generation fruit' together with sea buckthorn and raspberry.
Anthocyanidin is also called anthocyanidin, is a main color substance in plant flowers and fruits, is known as the 7 th most essential nutrient of human body after water, protein, fat, sugar, vitamin and mineral substances, and becomes the pigment with the most development prospect in natural pigments. The mulberry anthocyanin has been listed as a food additive variety which is approved by public notice of the health department due to the characteristics of high extraction rate, stable structure and the like, and is widely applied to the fields of food and health care products. The mulberry anthocyanin mainly comprises: cyanidin-3-O-glucoside, cyanidin-3-O-rutinoside, pelargonidin-3-O-glucoside, pelargonidin-3-O-rutinoside, etc.
In addition, the mulberry contains polyphenols such as gallic acid, protocatechuic acid, caffeic acid, syringic acid, cinnamic acid, ferulic acid, vanillic acid and coumaric acid, and these compounds have the effects of resisting arteriosclerosis, reducing cholesterol, resisting oxidation and resisting radiation.
The mulberry also contains various amino acids, wherein 6 amino acids such as threonine, lysine, valine, methionine, tryptophan, isoleucine and the like are necessary amino acids for human bodies, and the content of the total amino acids of the mulberry is 6-8 times higher than that of grapes, bananas, pears and oranges. The mulberry contains multiple vitamins such as VB1, VB2, VB3, VB5, VB6, VC, VE and the like, wherein the content of VC is the highest. Besides polysaccharides, the saccharide components in mulberry include fructose, glucose and sucrose, which are easily absorbed by human body.
China is the earliest country for breeding mulberry silkworms in the world, the cultivation of mulberry has a history of more than four thousand years, and the variety, variety and yield of mulberry are the top of the world. The mulberry resources in China are rich, and a plurality of methods for extracting anthocyanin from mulberries are provided. However, anthocyanin is only one of the active ingredients with economic value in mulberries, and if anthocyanin in mulberries is extracted and separated, and other ingredients are discarded as waste residues and waste materials, huge waste of resources is undoubtedly caused, so that environmental pollution is increased, and the production and processing cost is high. Therefore, the comprehensive utilization of mulberry resources should be solved early.
CN102212053A discloses a mulberry anthocyanin extraction method, which takes mulberry as a raw material, and comprises the steps of enzymolysis of cellulase and pectinase by ultrasound, extraction of deoxyhydrochloric acid aqueous solution at 75 ℃, flocculation of polymeric ferric sulfate, filtration, macroporous resin adsorption, nanofiltration membrane filtration of eluent and the like, thus obtaining the anthocyanin product with the highest product purity of 32%. In the method, whether the ultrasonic wave has promotion effect on the enzymolysis of the mulberry under the condition is uncertain, the anthocyanin is degraded due to overhigh extraction temperature, and partial anthocyanin is likely to be precipitated in the flocculation process of polymeric ferric sulfate, so that the yield of the mulberry anthocyanin obtained by the method is low.
CN102659743A discloses a method for extracting and refining anthocyanin from mulberry, which comprises the steps of taking fresh mulberry as a raw material, carrying out heat preservation extraction by acid water or acidic alcohol water solution, filtering, carrying out reduced pressure concentration, carrying out adsorption by macroporous adsorption resin, resolving aqueous alcohol solution, concentrating, carrying out spray drying and the like to obtain a mixture of anthocyanin and procyanidine. The method adopts spray drying mode, and can cause anthocyanin to degrade due to overhigh temperature.
CN104961783A discloses a method for effectively extracting anthocyanin and anthocyanin, which comprises the steps of taking cowberry, blackcurrant, blueberry, mulberry and black rice as raw materials, stirring and extracting by using an ethanol solution, concentrating under reduced pressure, refining by using macroporous adsorption resin, eluting by using ethanol, concentrating, spray drying and the like to obtain an extract containing anthocyanin and anthocyanin. The method adopts spray drying mode, and can cause anthocyanin to degrade due to overhigh temperature.
CN105524035A discloses a method for preparing mulberry anthocyanin, which comprises the steps of taking mulberries as raw materials, extracting with an alkaline aqueous solution containing a natural antioxidant, acidifying, flocculating, adsorbing by cation exchange resin, eluting with an acidic solution, concentrating under reduced pressure, spray drying and the like to obtain a mulberry anthocyanin product. Anthocyanins are extremely unstable in alkaline environments and flocculation and spray drying can lead to degradation of anthocyanins.
CN105949164A discloses a mulberry anthocyanin extraction method, which comprises the steps of pulping fresh mulberries as a raw material, acidifying with hydrochloric acid and stirring and leaching with ethanol, centrifuging, concentrating, extracting with ethyl acetate, carrying out macroporous resin adsorption column chromatography, eluting with ethanol, carrying out reduced pressure concentration and the like to obtain the mulberry anthocyanin. The method uses too much inflammable and explosive organic solvent, and is not suitable for industrial production.
CN106954773A discloses a processing method for comprehensively utilizing mulberry juice, which takes fresh mulberry fruits as raw materials, and the anthocyanin and concentrated, fermented and decolored mulberry juice are obtained through the steps of sorting, cleaning, squeezing, rough filtering, sterilization, enzymolysis, centrifugation, ultrafiltration, preconcentration, resin adsorption, water washing, anthocyanin elution, vacuum concentration, freeze drying, fermentation and the like. The method has low extraction rate of anthocyanidin.
The methods all have a common defect that only anthocyanin or anthocyanin active ingredients in the mulberry can be obtained, other natural active ingredients in the mulberry are not extracted and utilized, and the comprehensive and full utilization of natural resources is not realized.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art and provide the method for continuously extracting and separating the natural active ingredients from the mulberry, which has the advantages of high product yield, high active ingredient content and simple process and can continuously extract the natural active ingredients.
The technical scheme for solving the technical problems is that the method for continuously extracting and separating various natural active ingredients from the mulberry comprises the following steps:
(1) crushing raw materials, and leaching in cold water: crushing a mulberry raw material by using a crusher, adding cold water containing an anthocyanin protective agent, stirring, leaching, filtering, and collecting filtrate; obtaining cold water leaching liquor;
(2) centrifuging: centrifuging the cold water leaching liquor obtained in the step (1), and collecting a centrifugate;
(3) adsorption by macroporous adsorption resin: passing the centrifugate obtained in the step (2) through a macroporous adsorption resin column, and collecting effluent liquid on the column on the macroporous adsorption resin column for later use; after the column is loaded, washing the macroporous adsorption resin column to be slightly acidic by using pure water;
(4) and (3) separating anthocyanin: eluting the macroporous adsorption resin column which is washed to be slightly acidic in the step (3) by using low-alcohol to obtain low-alcohol eluent; concentrating the low-alcohol eluent under reduced pressure, and performing microwave drying to obtain an anthocyanin product;
(5) and (3) separation of polyphenol: eluting the macroporous adsorption resin column in the step (4) by using high ethanol to obtain high ethanol eluent; concentrating the high-alcohol eluent under reduced pressure, and performing microwave drying to obtain polyphenol products;
(6) desalting and decoloring: enabling the effluent liquid of the macroporous adsorption resin column upper column obtained in the step (3) to pass through a cation exchange resin column-anion exchange resin column connected in series, and collecting the effluent liquid of the cation exchange resin column-anion exchange resin column upper column; concentrating the effluent liquid on the cation exchange resin column and the anion exchange resin column under reduced pressure to obtain a decolorized concentrated mulberry juice product;
(7) separation of total amino acids: eluting the cation exchange resin column after the column is loaded in the step (6) by using dilute ammonia water, and collecting eluent; and (4) concentrating the eluent under reduced pressure, and drying by microwave to obtain a total amino acid product.
Further, in the step (1), the temperature of the cold water is 0-15 ℃; the anthocyanin protective agent is hydrosulfite, and the concentration of the anthocyanin protective agent in cold water is 0.05-0.5%.
Further, the bisulfite is sodium bisulfite, potassium bisulfite, calcium bisulfite, or ammonium bisulfite.
The purpose of using the anthocyanin protective agent is to prevent the anthocyanin from being oxidized and degraded in the processes of extraction, centrifugation and column loading. If the concentration of the protective agent is too low (the dosage is too small), the purpose of preventing the anthocyanin from being oxidized and degraded cannot be achieved; if the concentration of the protective agent is too high (too much amount), the material is wasted, and the burden of the subsequent desalting step is increased.
Further, in the step (1), stirring and leaching are carried out for 2 times, the amount of cold water used for the first time is 8-10 times of the weight of the mulberry raw material, the amount of cold water used for the second time is 5-8 times of the weight of the mulberry raw material, and the stirring and extracting time is 2-4 hours for the first time and 1-3 hours for the second time; the filtrates obtained by 2 times of leaching and filtration are combined.
The extraction with cold water under stirring is aimed at preventing the degradation of various active ingredients due to the over-high extraction temperature. The purpose of leaching twice is to ensure that various water-soluble active ingredients in the mulberry are thoroughly leached.
Further, in the step (2), the centrifugation is sedimentation type centrifugation, and the separation factor is 2000-5000.
The purpose of centrifugation is to remove water insoluble substances such as fine raw material particles, silt, plant fibers and the like in the cold water leaching liquor, so that the feed liquid is clarified. If the separation factor of the centrifuge is too small, the solid-liquid separation is insufficient, so that the raw material liquid on the macroporous resin column is turbid, and the adsorption and desorption are not facilitated; if the separation factor of the centrifugal machine is too large, the parameter requirement of the equipment is improved, and the input cost of the equipment is increased.
Further, in the step (3), the model of the macroporous adsorption resin is DM21, DM21D, DM28, LK2MG, DM-8 or AB-8; the height-diameter ratio of the macroporous adsorption resin column is 1-5: 1; the dosage of the resin is 0.5-3.0 times (L/kg) of the weight of the mulberry raw material; the flow rate of the upper column is 0.5-2.0 BV/h.
The macroporous adsorption resin column is used for adsorbing and enriching mulberry anthocyanin and mulberry polyphenol in the centrifugate on the macroporous adsorption resin. If the using amount of the macroporous adsorption resin is too small, the flow rate of the macroporous adsorption resin on the column is too high or the height-diameter ratio is too small, the mulberry anthocyanin and the mulberry polyphenol cannot be fully adsorbed; if the dosage of the macroporous absorption resin is too much, the flow rate of the macroporous absorption resin on the column is too slow or the height-diameter ratio is too large, the production period is prolonged and the production cost is increased.
Further, in the step (3), the amount of the pure water is 3-4 BV, and the flow rate of the washing is 1-2 BV/h.
The purpose of the water washing is to remove impurities such as salts and sugars which cannot be adsorbed in the resin column.
Further, in the step (4), the volume concentration of the low-alcohol ethanol is 30-40%; the dosage of the low alcohol is 2-3 BV; the flow rate of low-alcohol elution is 1-2 BV/h.
The purpose of low-alcohol elution is to elute the mulberry anthocyanidin adsorbed on the macroporous adsorption resin. If the volume concentration of the low-alcohol ethanol is too low, the dosage is too small or the elution flow rate is too high, the anthocyanin cannot be completely eluted, and the yield of the anthocyanin is low; if the volume concentration of the low-alcohol ethanol is too high, the dosage is too high or the elution flow rate is too low, part of the mulberry polyphenol can be eluted, so that the purity (content) of the anthocyanin product is low, and the yield of the mulberry polyphenol is low.
Further, in the step (5), the volume concentration of the high-ethanol is 55-70%, the using amount of the high-ethanol is 2-3 BV, and the flow rate of the high-ethanol elution is 1-2 BV/h.
The purpose of the high ethanol elution is to elute the mulberry polyphenol adsorbed on the macroporous adsorbent resin. If the volume concentration of the high-alcohol is too low, the dosage is too small or the elution flow rate is too high, the polyphenol cannot be completely eluted, and the yield of the polyphenol is low; if the volume concentration of the high-alcohol is too high, the dosage is too high or the elution flow rate is too low, the energy and the materials are wasted.
Further, in the step (4), the step (5) and the step (7), the temperature of the reduced pressure concentration is 55-60 ℃, the vacuum degree is-0.08-0.09 MPa, and the concentration is carried out until the solid content is 15-25%; the temperature of the microwave drying is 50-60 ℃, the vacuum degree is-0.08-0.09 MPa, and the microwave frequency is 2450-2550 MHz.
Further, in the step (6), the cation exchange resin is a strongly acidic styrene-based cation exchange resin, and the type of the cation exchange resin is 001 × 7, 001 × 8, 001 × 12, or 001 × 16.
Further, in the step (6), the height-diameter ratio of the cation exchange resin column is 3-6: 1, and the flow rate of the material passing through the cation exchange resin column is 1-2 BV/h; the resin dosage of the cation exchange resin is 0.1-0.5 time (L/kg) of the weight of the mulberry raw material.
The purpose of using the cation exchange resin column is to desalt and adsorb amino acids in the column effluent on the macroporous adsorbent resin column. If the amount of the cation exchange resin used is too small, the aspect ratio of the cation exchange resin column is too small, or the flow rate of the material passing through the cation exchange resin column is too high, the above-mentioned object cannot be sufficiently achieved. If the dosage of the cation exchange resin is too much, the height-diameter ratio of the cation exchange resin column is too large or the flow rate of the material passing through the cation exchange resin column is too slow, the waste of energy or material is caused.
Further, in the step (6), the anion exchange resin is a macroporous strongly basic anion exchange resin; the cation exchange resin is preferably of the type D941, D945, D285 or 330.
Further, in the step (6), the height-diameter ratio of the anion exchange resin column is 3-6: 1; the flow rate of the materials passing through the anion exchange resin column is 1-2 BV/h; the resin dosage of the anion exchange resin is 0.1-0.5 time (L/kg) of the weight of the mulberry raw material.
The purpose of using the anion exchange resin column is to decolor and remove impurities so as to improve the purity of the decolored concentrated juice of the mulberry. If the amount of the anion exchange resin used is too small, the aspect ratio of the anion exchange resin column is too small, or the flow rate of the material passing through the anion exchange resin column is too high, the above-mentioned objects cannot be sufficiently achieved. If the dosage of the anion exchange resin is too much, the height-diameter ratio of the anion exchange resin column is too large or the flow rate of the material passing through the anion exchange resin column is too slow, the waste of energy or material is caused.
Further, in the step (6), the temperature of the reduced pressure concentration is 60-70 ℃, the vacuum degree is-0.08 to-0.09 MPa, and the concentration is carried out until the sugar degree is 55-65 Brix; the concentration of the dilute ammonia water is 0.5-1.0 mol/L, the using amount of the dilute ammonia water is 3-5 BV, and the eluting flow rate of the dilute ammonia water is 1-2 BV/h.
The purpose of elution with dilute ammonia water is to elute the mulberry amino acid adsorbed on the cation exchange resin. If the concentration of the dilute ammonia water is too low, the dosage is too small or the elution flow rate is too high, the amino acid cannot be completely eluted, so that the yield of the amino acid is low; if the concentration of the dilute ammonia water is too high, the dosage is too high or the elution flow rate is too low, the waste of energy and materials is caused.
In the present invention, 1BV =1 column volume.
The principle of the method of the invention is as follows: the low-temperature cold water extraction containing the anthocyanin protective agent can fully leach water-soluble ingredients in the mulberry raw material and ensure that the extracted natural active ingredients have stable properties and are not oxidized and degraded. The mulberry anthocyanin and the mulberry polyphenol in the water-soluble components are adsorbed in the macroporous adsorption resin through selective enrichment of the macroporous adsorption resin, and then the mulberry anthocyanin and the mulberry polyphenol are sequentially eluted from the macroporous adsorption resin column in a gradient elution mode according to different polarities of the mulberry anthocyanin and the mulberry polyphenol, so that the separation of the mulberry anthocyanin and the mulberry polyphenol is realized. Other water-soluble components including amino acids, polysaccharides, sucrose, fructose, glucose, vitamins, inorganic salts, etc. are not adsorbed by the macroporous adsorbent resin and exist in the effluent of the column on the macroporous adsorbent resin column. Desalting and decoloring the column effluent on the macroporous adsorption resin column by using a cation-anion exchange resin column to obtain an important byproduct, namely mulberry decolored concentrated juice. The amino acid is enriched by cation exchange resin, and is eluted by ammonia water, concentrated and dried to obtain the mulberry amino acid product.
Compared with the prior art, the invention has the following beneficial effects:
(1) the anthocyanin content of the mulberry anthocyanin product obtained by the invention is 65.49%, and the yield is 95.27%; the polyphenol content of the mulberry polyphenol product reaches 85.72 percent, and the yield reaches 93.48 percent; the amino acid content of the mulberry amino acid product reaches up to 71.43 percent, and the yield reaches 91.39 percent.
(2) The method can simultaneously extract three natural active ingredients in the mulberry, realizes full and comprehensive utilization of mulberry resources, and has the advantages of simple process, strong operability, low requirement on equipment, low production cost, safety, greenness, environmental protection and suitability for industrial production.
(3) The invention comprehensively treats the effluent liquid on the macroporous adsorption resin column, which is usually used as waste liquid in the actual production, so that the decolorized concentrated juice of mulberry rich in polysaccharide, sucrose, fructose, glucose and vitamins is obtained, the added value of the product is greatly improved, the environmental pollution is reduced, and the resource utilization rate is improved.
Detailed Description
The present invention will be further described with reference to the following examples.
The mulberry raw material used in the embodiment of the invention is purchased from Sichuan, wherein the anthocyanin, the polyphenol and the amino acid are respectively 1.83%, 5.30% and 0.67% in percentage by mass; the macroporous adsorption resin and the ion exchange resin used in the embodiment of the invention are purchased from Aimeikejian (China) biological medicine Co., Ltd; the starting materials or chemicals used in the examples of the present invention are, unless otherwise specified, commercially available in a conventional manner.
In the embodiment of the invention, the content of mulberry anthocyanins (containing cyanidin-3-O-glucoside, cyanidin-3-O-rutinoside, pelargonidin-3-O-glucoside and pelargonidin-3-O-rutinoside) is determined by adopting a High Performance Liquid Chromatography (HPLC) external standard method, the content of mulberry polyphenol is determined by adopting a ferrous tartrate colorimetric method, and the content of mulberry amino acid (total) is determined by adopting a ninhydrin color rendering method.
Example 1
The embodiment comprises the following steps:
(1) crushing raw materials, and leaching in cold water: taking 100kg of dried mulberry raw material, crushing the mulberry raw material by using a crusher until the particle size is 1-2 mm, adding 1000L of cold water (containing sodium bisulfite with the mass concentration of 0.3%) with the temperature of 8 ℃, stirring and leaching for 4 hours, carrying out coarse filtration, and collecting filter residues and filtrate; stirring and leaching the filter residue with 600L of the same cold water for 2 hours again, coarsely filtering, and collecting the filtrate; then combining the two filtrates to obtain a cold water leaching liquor;
(2) centrifuging: centrifuging the cold water leaching liquor obtained in the step (1) by using a sedimentation type centrifuge with a separation factor of 3200, and collecting a centrifugate;
(3) adsorption by macroporous adsorption resin: enabling the centrifugate obtained in the step (2) to pass through a macroporous adsorption resin column (the model of the macroporous adsorption resin is DM21, the height-diameter ratio of the macroporous adsorption resin column is 4:1, the using amount of the macroporous adsorption resin is 150L, and the flow rate of the macroporous adsorption resin column is 1.5 BV/h), and collecting the effluent liquid of the macroporous adsorption resin column on the column for standby; after the column loading, washing the macroporous adsorption resin column to be slightly acidic by using 3BV of pure water at the flow rate of 1.5 BV/h;
(4) and (3) separating anthocyanin: eluting the macroporous adsorption resin column which is washed to be slightly acidic in the step (3) by using low-alcohol with the volume concentration of 32% and the flow rate of elution being 2BV/h, concentrating the low-alcohol eluent under reduced pressure under the conditions that the temperature is 60 ℃ and the vacuum degree is-0.08 MPa until the solid content is 20%, and then carrying out microwave drying on the concentrated solution under the conditions that the temperature is 60 ℃, the vacuum degree is-0.08 MPa and the microwave frequency is 2450MHz to obtain 2.70kg of mulberry anthocyanin product;
(5) and (3) separation of polyphenol: eluting the macroporous adsorption resin column eluted in the step (4) by using high ethanol with the volume concentration of 70% and the flow rate of elution being 1BV/h at 2.5 BV, concentrating the high ethanol eluent under reduced pressure under the conditions that the temperature is 60 ℃ and the vacuum degree is-0.08 MPa until the solid content is 22%, and then carrying out microwave drying on the concentrated solution under the conditions that the temperature is 60 ℃, the vacuum degree is-0.08 MPa and the microwave frequency is 2450MHz to obtain 5.73kg of mulberry polyphenol products;
(6) desalting and decoloring: enabling the effluent liquid of the macroporous adsorption resin column in the step (3) to pass through a cation-anion exchange resin column (the type of the cation exchange resin is 001 multiplied by 16, the using amount of the cation exchange resin is 20L, the height-diameter ratio of the cation exchange resin column is 4:1, the flow rate of the material passing through the cation exchange resin column is 1BV/h, the type of the anion exchange resin is D941, the using amount of the anion exchange resin is 20L, the height-diameter ratio of the anion exchange resin column is 4:1, the flow rate of the material passing through the anion exchange resin column is 1 BV/h), collecting the effluent liquid of the cation-anion exchange resin column, and concentrating under reduced pressure at the temperature of 70 ℃ and the vacuum degree of-0.08 MPa until the sugar degree is 65Brix to obtain 30.77kg of the decolorized concentrated mulberry juice product;
(7) separation of total amino acids: eluting the cation exchange resin column eluted in the step (6) with dilute ammonia water of 4BV and 0.7mol/L concentration at the eluting flow rate of 1.5BV/h, concentrating the dilute ammonia water eluent under reduced pressure, and drying by microwave to obtain 0.85kg of mulberry total amino acid product.
The content of anthocyanin in the mulberry anthocyanin product obtained in the embodiment is 64.57% and the yield of mulberry anthocyanin is 95.27% as determined by a High Performance Liquid Chromatography (HPLC) external standard method; according to the determination of a ferrous tartrate colorimetric method, the polyphenol content of the mulberry polyphenol product obtained in the embodiment is 82.27%, and the yield of the mulberry polyphenol is 88.94%; the amino acid content of the mulberry amino acid product obtained in the example is 71.43% and the yield of total amino acids of the mulberry is 90.62% as determined by a ninhydrin color development method.
Example 2
The embodiment comprises the following steps:
(1) crushing raw materials, and leaching in cold water: taking 100kg of dried mulberry raw material, crushing the mulberry raw material by using a crusher until the particle size is 1-2 mm, adding 800L of cold water (containing potassium bisulfite and the concentration of 0.1%) with the temperature of 5 ℃, stirring and leaching for 3.5 hours, carrying out coarse filtration, and collecting filter residues and filtrate; stirring and leaching the filter residue with 700L of the same cold water for 3 hours again, coarsely filtering, and collecting the filtrate; then combining the two filtrates to obtain a cold water leaching liquor;
(2) centrifuging: centrifuging the cold water leaching liquor obtained in the step (1) by using a decanter centrifuge with the separation factor of 4000, and collecting a centrifugate;
(3) adsorption by macroporous adsorption resin: enabling the centrifugate obtained in the step (2) to pass through a macroporous adsorption resin column (the model of the macroporous adsorption resin is DM21D, the height-diameter ratio of the macroporous adsorption resin column is 3.5:1, the using amount of the macroporous adsorption resin is 200L, and the flow rate of the macroporous adsorption resin column is 2.0 BV/h), and collecting the effluent liquid of the macroporous adsorption resin column; after the column loading, washing the macroporous absorption resin column to be slightly acidic by using 3.5 BV of pure water at the flow rate of 1.5 BV/h;
(4) and (3) separating anthocyanin: eluting the macroporous adsorption resin column which is washed to be slightly acidic in the step (3) by using low-alcohol with the volume concentration of 35% and the flow rate of elution being 1.5BV/h, concentrating the low-alcohol eluent under reduced pressure under the conditions that the temperature is 56 ℃ and the vacuum degree is-0.09 MPa until the solid content is 18%, and then carrying out microwave drying on the concentrated solution under the conditions that the temperature is 56 ℃, the vacuum degree is-0.09 MPa and the microwave frequency is 2450MHz to obtain 2.69kg of mulberry anthocyanin products;
(5) and (3) separation of polyphenol: eluting the macroporous adsorption resin column eluted in the step (4) by using high ethanol with the volume concentration of 65% and the flow rate of elution being 1.5BV/h at 3BV, concentrating the high ethanol eluent under reduced pressure under the conditions that the temperature is 58 ℃ and the vacuum degree is-0.09 MPa until the solid content is 20%, and then performing microwave drying on the concentrated solution under the conditions that the temperature is 58 ℃, the vacuum degree is-0.09 MPa and the microwave frequency is 2450MHz to obtain 5.78kg of mulberry polyphenol product;
(6) desalting and decoloring: enabling the effluent liquid of the macroporous adsorption resin column in the step (3) to pass through a cation-anion exchange resin column (the type of the cation exchange resin is 001 multiplied by 12, the using amount of the cation exchange resin is 30L, the height-diameter ratio of the cation exchange resin column is 5:1, the flow rate of the material passing through the cation exchange resin column is 1.5BV/h, the type of the anion exchange resin is D945, the using amount of the anion exchange resin is 30L, the height-diameter ratio of the anion exchange resin column is 5:1, the flow rate of the material passing through the anion exchange resin column is 1.5 BV/h), collecting the effluent liquid of the cation-anion exchange resin column, and concentrating under reduced pressure under the conditions that the temperature is 68 ℃ and the vacuum degree is-0.08 MPa until the sugar degree is 60 Brix to obtain 32.67kg of the concentrated decolorized mulberry juice;
(7) separation of total amino acids: eluting the cation exchange resin column eluted in the step (6) with dilute ammonia water of 5BV and 0.6mol/L concentration at the elution flow rate of 2BV/h, concentrating the dilute ammonia water eluent under reduced pressure, and drying by microwave to obtain 0.88kg of mulberry total amino acid product.
The content of the anthocyanin in the mulberry anthocyanin product obtained in the embodiment is 63.19% and the yield of the mulberry anthocyanin is 92.89% as determined by a High Performance Liquid Chromatography (HPLC) external standard method; according to the determination of a ferrous tartrate colorimetric method, the polyphenol content of the mulberry polyphenol product obtained in the embodiment is 85.72%, and the yield of the mulberry polyphenol is 93.48%; the amino acid content of the mulberry amino acid product obtained in the example is 69.58% and the yield of total amino acids of mulberry is 91.39% as determined by a ninhydrin color development method.
Example 3
The embodiment comprises the following steps:
(1) crushing raw materials, and leaching in cold water: taking 100kg of dried mulberry raw material, crushing the mulberry raw material by using a crusher until the particle size is 1-2 mm, adding 900L of cold water (containing calcium hydrogen sulfite and the concentration of 0.05%) with the temperature of 10 ℃, stirring and leaching for 3 hours, carrying out coarse filtration, and collecting filter residues and filtrate; stirring and leaching the filter residue with 800L of the same cold water for 2.5 hours again, coarsely filtering, and collecting the filtrate; then combining the two filtrates to obtain a cold water leaching liquor;
(2) centrifuging: centrifuging the cold water leaching liquor obtained in the step (1) by using a sedimentation type centrifuge with a separation factor of 3500, and collecting a centrifugate;
(3) adsorption by macroporous adsorption resin: enabling the centrifugate obtained in the step (2) to pass through a macroporous adsorption resin column (the model of the macroporous adsorption resin is LK2MG, the height-diameter ratio of the macroporous adsorption resin column is 5:1, the using amount of the macroporous adsorption resin is 180L, and the flow rate of the macroporous adsorption resin column is 1.0 BV/h), and collecting the effluent liquid of the macroporous adsorption resin column; after the column loading is finished, washing the macroporous adsorption resin column to be slightly acidic by using 4BV of pure water at the flow rate of 2 BV/h;
(4) and (3) separating anthocyanin: eluting the macroporous adsorption resin column which is washed to be slightly acidic in the step (3) by using low-alcohol with the volume concentration of 30% and the flow rate of elution being 1BV/h, concentrating the low-alcohol eluent under reduced pressure under the conditions of the temperature of 58 ℃ and the vacuum degree of minus 0.08MPa until the content of solid matters is 23%, and then carrying out microwave drying on the concentrated solution under the conditions of the temperature of 58 ℃, the vacuum degree of minus 0.08MPa and the microwave frequency of 2450MHz to obtain 2.63kg of the mulberry anthocyanin product;
(5) and (3) separation of polyphenol: eluting the macroporous adsorption resin column eluted in the step (4) by using high ethanol with the volume concentration of 60% and the flow rate of elution being 1.5BV/h and with the volume concentration of 3BV, concentrating the high ethanol eluent under the conditions of the temperature of 60 ℃ and the vacuum degree of minus 0.08MPa until the solid content is 18%, and then carrying out microwave drying on the concentrated solution under the conditions of the temperature of 60 ℃, the vacuum degree of minus 0.08MPa and the microwave frequency of 2450MHz to obtain 5.46kg of mulberry polyphenol product;
(6) desalting and decoloring: enabling the effluent liquid of the macroporous adsorption resin column in the step (3) to pass through a cation-anion exchange resin column (the type of cation exchange resin is 001 multiplied by 7, the dosage of the cation exchange resin is 25L, the height-diameter ratio of the cation exchange resin column is 6:1, the flow rate of the material passing through the cation exchange resin column is 2BV/h, the type of anion exchange resin is D285, the dosage of the anion exchange resin is 25L, the height-diameter ratio of the anion exchange resin column is 6:1, the flow rate of the material passing through the anion exchange resin column is 2 BV/h), collecting the effluent liquid of the cation-anion exchange resin column, and concentrating under the conditions that the temperature is 65 ℃ and the vacuum degree is-0.09 MPa until the sugar degree is 63 Brix to obtain 31.43kg of the mulberry decolorized concentrated juice product;
(7) separation of total amino acids: eluting the cation exchange resin column eluted in the step (6) with dilute ammonia water of 4.5BV and 0.9mol/L concentration at the elution flow rate of 1BV/h, concentrating the dilute ammonia water eluent under reduced pressure, and performing microwave drying to obtain 0.89kg of mulberry total amino acid product.
The content of the anthocyanin in the mulberry anthocyanin product obtained in the embodiment is 65.49% and the yield of the mulberry anthocyanin is 94.12% as determined by a High Performance Liquid Chromatography (HPLC) external standard method; according to the determination of a ferrous tartrate colorimetric method, the polyphenol content of the mulberry polyphenol product obtained in the embodiment is 83.50%, and the yield of the mulberry polyphenol is 86.02%; the amino acid content of the mulberry amino acid product obtained in the example is 68.74% and the yield of total amino acids of mulberry is 91.31% as determined by a ninhydrin color development method.
Comparative example 1
Comparative example 1 is compared with example 1 except that sodium bisulfite was not added to the cold water used in step (1), and other raw materials and extraction conditions were the same as in example 1.
The content of anthocyanin in the obtained mulberry anthocyanin product is 59.31 percent and the yield of the mulberry anthocyanin is 85.76 percent, which are determined by a High Performance Liquid Chromatography (HPLC) external standard method; according to the determination of a ferrous tartrate colorimetric method, the polyphenol content of the mulberry polyphenol product obtained in the embodiment is 81.37%, and the yield of the mulberry polyphenol is 87.56%; the amino acid content of the mulberry amino acid product obtained in the example is 69.83% and the yield of total mulberry amino acids is 89.74% as determined by a ninhydrin color development method.
Comparative example 2
Comparative example 2 is different from example 1 only in that the concentration of sodium bisulfite in cold water used in step (1) is 0.02%, and other raw materials and extraction conditions are the same as those of example 1.
The anthocyanin content of the obtained mulberry anthocyanin product is 60.18% and the yield of the mulberry anthocyanin is 86.82% as determined by a High Performance Liquid Chromatography (HPLC) external standard method; according to the determination of a ferrous tartrate colorimetric method, the polyphenol content of the mulberry polyphenol product obtained in the embodiment is 84.37%, and the yield of the mulberry polyphenol is 91.65%; the amino acid content of the mulberry amino acid product obtained in the example is 68.68% and the yield of total mulberry amino acids is 90.52% as determined by a ninhydrin color development method.
The above embodiments are specific illustrations of some possible embodiments of the invention, and these embodiments are not intended to limit the scope of the invention, and all equivalent implementations or modifications that do not depart from the scope of the invention are intended to be included within the scope of the claims of the present application.

Claims (10)

1. The method for continuously extracting and separating various natural active ingredients from the mulberries is characterized by comprising the following steps:
(1) crushing raw materials, and leaching in cold water: crushing a mulberry raw material by using a crusher, adding cold water containing an anthocyanin protective agent, stirring, leaching, filtering, and collecting filtrate to obtain cold water leaching liquor;
(2) centrifuging: centrifuging the cold water leaching liquor obtained in the step (1), and collecting a centrifugate;
(3) adsorption by macroporous adsorption resin: passing the centrifugate obtained in the step (2) through a macroporous adsorption resin column, and collecting effluent liquid on the column on the macroporous adsorption resin column for later use; after the column is loaded, washing the macroporous adsorption resin column to be slightly acidic by using pure water;
(4) and (3) separating anthocyanin: eluting the macroporous adsorption resin column which is washed to be slightly acidic in the step (3) by using low-alcohol to obtain low-alcohol eluent; concentrating the low-alcohol eluent under reduced pressure, and performing microwave drying to obtain an anthocyanin product;
(5) and (3) separation of polyphenol: eluting the macroporous adsorption resin column in the step (4) by using high ethanol to obtain high ethanol eluent; concentrating the high-alcohol eluent under reduced pressure, and performing microwave drying to obtain polyphenol products;
(6) desalting and decoloring: enabling the effluent liquid of the macroporous adsorption resin column upper column obtained in the step (3) to pass through a cation exchange resin column-anion exchange resin column connected in series, and collecting the effluent liquid of the cation exchange resin column-anion exchange resin column upper column; concentrating the effluent liquid on the cation exchange resin column and the anion exchange resin column under reduced pressure to obtain a decolorized concentrated mulberry juice product;
(7) separation of total amino acids: eluting the cation exchange resin column after the column is loaded in the step (6) by using dilute ammonia water, and collecting eluent; and (4) concentrating the eluent under reduced pressure, and drying by microwave to obtain a total amino acid product.
2. The method for continuously extracting and separating natural active ingredients from mulberry as claimed in claim 1, wherein in the step (1), the temperature of the cold water is 0-15 ℃; the anthocyanin protective agent is bisulfite, and the concentration of the protective agent in cold water is 0.05-0.5%; the bisulfite is preferably sodium bisulfite, potassium bisulfite, calcium bisulfite, or ammonium bisulfite.
3. The method for continuously extracting and separating multiple natural active ingredients from mulberry according to claim 1 or 2, wherein in the step (1), the stirring extraction is carried out for 2 times, the amount of cold water used for the first time is 8-10 times of the weight of the mulberry raw material, and the amount of cold water used for the second time is 5-8 times of the weight of the mulberry raw material; stirring and extracting for 2-4 hours for the first time and 1-3 hours for the second time; merging the filtrates obtained by leaching and filtering for 2 times; in the step (2), the centrifugation is sedimentation type centrifugation, and the separation factor is 2000-5000.
4. The method for continuously extracting and separating multiple natural active ingredients from the mulberry according to any one of claims 1 to 3, wherein in the step (3), the type of the macroporous adsorption resin is DM21, DM21D, DM28, LK2MG, DM-8 or AB-8, the height-diameter ratio of a macroporous adsorption resin column is 1-5: 1, the amount of the resin is 0.5-3.0 times (L/kg) of the weight of the mulberry raw material, and the flow rate of the resin on the column is 0.5-2.0 BV/h; the amount of the pure water is 3-4 BV, and the flow rate of the washing is 1-2 BV/h.
5. The method for continuously extracting and separating multiple natural active ingredients from mulberry according to any one of claims 1 to 4, wherein in the step (4), the volume concentration of the low-alcohol-content ethanol is 30-40%, the dosage of the low-alcohol-content ethanol is 2-3 BV, and the flow rate of elution of the low-alcohol-content ethanol is 1-2 BV/h.
6. The method for continuously extracting and separating multiple natural active ingredients from mulberry according to any one of claims 1 to 5, wherein in the step (5), the volume concentration of the high-grade ethanol is 55-70%, the using amount of the high-grade ethanol is 2-3 BV, and the flow rate of the high-grade ethanol elution is 1-2 BV/h.
7. The method for continuously extracting and separating multiple natural active ingredients from mulberry according to any one of claims 1 to 6, wherein in the step (4), the step (5) and the step (7), the temperature of the reduced pressure concentration is 55-60 ℃, the vacuum degree is-0.08-0.09 MPa, and the concentration is carried out until the solid content is 15-25%; the temperature of the microwave drying is 50-60 ℃, the vacuum degree is-0.08-0.09 MPa, and the microwave frequency is 2450-2550 MHz.
8. The method for continuously extracting and separating multiple natural active ingredients from mulberry as claimed in any one of claims 1 to 7, wherein in the step (6), the cation exchange resin is a strongly acidic styrene cation exchange resin; the type of the cation exchange resin is preferably 001 × 7, 001 × 8, 001 × 12 or 001 × 16; the height-diameter ratio of the cation exchange resin column is preferably 3-6: 1, and the flow rate of the material passing through the cation exchange resin column is preferably 1-2 BV/h; the dosage of the cation exchange resin is preferably 0.1-0.5 time (L/kg) of the weight of the mulberry raw material.
9. The method for continuously extracting and separating multiple natural active ingredients from mulberry according to any one of claims 1 to 8, wherein in the step (6), the anion exchange resin is a macroporous strong-base anion exchange resin; the cation exchange resin is preferably D941, D945, D285 or 330; the height-diameter ratio of the anion exchange resin column is preferably 3-6: 1; the flow rate of the materials passing through the anion exchange resin column is preferably 1-2 BV/h; the resin dosage of the anion exchange resin is preferably 0.1-0.5 time (L/kg) of the weight of the mulberry raw material.
10. The method for continuously extracting and separating multiple natural active ingredients from mulberry according to any one of claims 1 to 9, wherein in the step (6), the temperature for reduced pressure concentration is 60 to 70 ℃, the vacuum degree is-0.08 to-0.09 MPa, and the concentration is carried out until the sugar degree is 55 to 65 Brix; the concentration of the dilute ammonia water is preferably 0.5-1.0 mol/L, the using amount of the dilute ammonia water is preferably 3-5 BV, and the eluting flow rate of the dilute ammonia water is preferably 1-2 BV/h.
CN202110732680.6A 2021-06-30 2021-06-30 Method for continuously extracting and separating multiple natural active ingredients from mulberries Pending CN113397169A (en)

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