CN105193863B - A kind of preparation method of high-purity seeweed polyphenol - Google Patents
A kind of preparation method of high-purity seeweed polyphenol Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of high-purity seeweed polyphenol, including the processing steps such as algal polysaccharides and the separation of seaweed slag, the enzymolysis broken wall of seaweed slag, the high efficiency extraction of seeweed polyphenol, the isolating and purifying of seeweed polyphenol, the acquisition of high-purity seeweed polyphenol, realize algal polysaccharides, seeweed polyphenol, seaweed slag full algae comprehensively utilize.
Description
Technical field
The present invention relates to the technical field of seeweed polyphenol more particularly to a kind of preparation methods of high-purity seeweed polyphenol.
Background technology
Seaweed is the main source of sea-plant polyphenol, and there are a great differences with Lu Yuan plant polyphenols for structure：Lu Yuanzhi
Object polyphenol is by gallic acid and to mix acid is spent to be derived；Seeweed polyphenol is then the derivative of phloroglucin.Studies have shown that seaweed
Polyphenol has special efficacy in anti-oxidant, improvement metabolic syndrome, prevention degenerative disease etc., and safe and non-toxic.Therefore, American-European state
Family's development and application of input huge fund implementation seeweed polyphenol in succession.High-purity seeweed polyphenol strong, medical value with bioactivity
The high, advantages such as stability is good, are the products of biomedicine field active demand.
However, since seeweed polyphenol is present in the bubble of the algae inside alginic cell, embedded by phycocolloid, cellulose even depth,
Conventional extraction techniques are difficult to obtain high yield, and production cost is high, and purity is relatively low.For example, Chinese invention patent application
CN102579508A《A kind of preparation method of sargassum fusifome brown algae polyphenols》, it is open using sargassum fusifome as raw material, it is carried using methanol heating
(40 DEG C) are taken, then use different solvents extraction and ultrafiltration retention means that brown algae polyphenols are prepared；Chinese invention patent application
CN102397300A《A kind of extracting method of brown algae polyphenols》, it is open using Fresh Laminaria Japonica, sargassum thunbergii, sargassum kjellmanianum Yendo as raw material, it uses
3 kinds of brown algae polyphenols are prepared in solvent extraction, macroporous resin purification, and yield is respectively 0.3 ‰, 2.5 ‰, 3 ‰；Middle promulgated by the State Council
Bright patent application CN103610704A《A kind of extracting method of brown algae polyphenols》, open to be with fresh Sargassum brown alga or kelp
Raw material is extracted in hot bath using organic solvent after broken, is obtained after macroporous resin purification, elution, concentration, freeze-drying
Brown algae polyphenols extract, yield are 2.5 ‰；Chinese invention patent application CN104382951A《A kind of extraction side of seeweed polyphenol
Method》, it is open using three kinds of chlorella pyrenoidosa, Euglena, salt algae algae as raw material, using ethyl alcohol as solvent, using microwave combined extraction
Technology obtains the polyphenol extract of 3 kinds of seaweed after extracting solution filtering through freeze-drying；Chinese invention patent mandate
CN102935093B《A kind of extracting method of seeweed polyphenol》, it is open using the seawood meal of 40 mesh as raw material, using microwave assisted aqueous extraction
Formulation extracts, and then obtains the polyphenol extract of purity 75% or so through macroporous resin purification；Chinese invention patent mandate
CN102166230B《The method of microwave radiation technology seeweed polyphenol》, it is open using seawood meal as raw material, with alcohol-acetone-water mixed solvent,
Seeweed polyphenol is extracted in conjunction with microwave technology, obtains seeweed polyphenol crude extract through filtering, being freeze-dried, recovery rate is up to 2.26%.
The above-mentioned method for preparing seeweed polyphenol lacks the comprehensive utilization to main components such as algins, serious waste of resources；It is above-mentioned simultaneously
The technology for preparing seeweed polyphenol there is problems：1) inferior separating effect, purity are low.Seeweed polyphenol easily with algin,
Albumen forms compound in the form of non-covalent bond, is difficult to be isolated in subsequent purification process, leads to returning for seeweed polyphenol
Yield is low；In addition, also containing a large amount of fat-soluble pigments in the seeweed polyphenol of extraction, traditional column chromatography technology, which cannot achieve, effectively to be divided
From causing the purity of product low.2) structure is destroyed big, and activity is low.Seeweed polyphenol is extremely unstable, oxidizable, in process
High temperature, alkaline ph values, oxygen etc. can destroy its bioactivity.Although microwave technology, ultrasound-assisted extraction technology can improve
The yield of seaweed ocean polyphenol, but extraction process will produce high temperature, in addition lacking effective protection measure, accelerate under the effect of the oxygen
The oxidation of ocean polyphenol, leads to loss of activity.3) production technology is complicated, of high cost.Currently used for the technique for processing seeweed polyphenol
Including crushing, extraction, centrifugation, filtering, upper prop, elution, resin regeneration, the repeatedly multiple working procedures such as concentration, dry；Conventional column chromatography
Purifying seeweed polyphenol must also be equipped with the equipment such as constant flow pump, glass column, collection device, cause the production time long, and equipment requirement is high,
Limit industrialized development.This is the key technology bottleneck for leading to seeweed polyphenol commercial application.
In view of this, the present inventor studies and devises a kind of preparation method of high-purity seeweed polyphenol, thus this case is produced
It is raw.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of high-purity seeweed polyphenol, including algal polysaccharides and seaweed slag
Separation, the enzymolysis broken wall of seaweed slag, the high efficiency extraction of seeweed polyphenol, the isolating and purifying of seeweed polyphenol, high-purity seeweed polyphenol
The processing steps such as acquisition, with realize algal polysaccharides, seeweed polyphenol, seaweed slag full algae comprehensively utilize.
To achieve the goals above, the technical scheme adopted by the invention to solve the technical problem is that：
A kind of preparation method of high-purity seeweed polyphenol, includes the following steps：
Step 1: the separation of algal polysaccharides and seaweed slag：The dry seaweed that water content is 20% is impregnated with tap water first,
Rinsing is beaten after removing silt impurity with beater；Seaweed slurry is sent into blender, and is starched by seaweed：Deionized water volume ratio is
1：5 are added deionized water, are stirred 30 minutes with 120 turns/min rotating speeds at room temperature；Seaweed slurry low speed centrifuge with 1000 turns/
The rotating speed of min centrifuges 5min, collects supernatant and seaweed slag respectively；Seaweed slag by above-mentioned steps and the stirring of condition agitated machine,
After centrifuge processing, supernatant and seaweed slag are collected respectively again；Merge supernatant twice, sea is obtained after spray-dried
Polysaccharides；Seaweed slag is collected, seeweed polyphenol is prepared for extraction；
Step 2: the enzymolysis broken wall of seaweed slag：It will be by cellulase and pectase by weight 1：The complex enzyme of 1 composition is pressed
Weight ratio is 1:1000 are added in the seaweed slag, hydrolyze 5h at room temperature, realize alginic cell wall broken wall；
Step 3: the high efficiency extraction of seeweed polyphenol：Seeweed polyphenol protective agent is dissolved in deionized water, then with food
Grade absolute ethyl alcohol is 1 by volume：4 mixing, and are added acetic acid by volume, make acetic acid final volume a concentration of 0.1%, after mixing
For the extracting solution of seeweed polyphenol；The extracting solution is 5 by volume/weight ratio with seaweed slag:1 carries out mixing, extracts at room temperature
1.5h centrifuges 5min with the rotating speed of 3000 turns/min, collects supernatant and seaweed slag respectively；Seaweed slag continues with the extracting solution
It repeats abovementioned steps and carries out second extraction, collect supernatant and seaweed slag respectively；Seaweed slag is used for feed addictive after drying
Raw material；Merge supernatant twice, for isolating and purifying for seeweed polyphenol；
Step 4: seeweed polyphenol isolates and purifies：By supernatant made from step 3 pour into the adsorption tank containing silica gel into
Row Static Adsorption decoloration 2h, the pigment of silica gel absorption are further used for preparing fucoxanthine active material；Then dense using depressurizing
After seeweed polyphenol extracting solution is concentrated into 50% volume by contracting method at 40 DEG C, resin is absorbed to seaweed using domestic XDA-7 macropores
Polyphenol carries out Solid Phase Extraction 2h；By XDA-7 macroreticular resins deionized water short rinse, except desaccharification, small peptide impurity；Then will
XDA-7 macroreticular resins impregnate 0.5h with food-grade anhydrous ethyl alcohol, and the seeweed polyphenol being adsorbed on macroreticular resin is eluted and dissolved
In ethyl alcohol, ethyl alcohol soak is obtained；
Step 5: the preparation of seeweed polyphenol：The ethyl alcohol soak is concentrated to dryness at 40 DEG C, it is true at 50 DEG C
The dry 2h of sky, obtains seeweed polyphenol product.
As the preferred embodiment of embodiment, the seaweed is kelp, undaria pinnitafida, the sacrificial dish of sheep, sargassum kjellmanianum Yendo, sargassum thunbergii and Gan Tai
At least one of.
As the preferred embodiment of embodiment, the seeweed polyphenol protective agent of the step 3 is for vitamin C or phytic acid or by tieing up
The compound of raw element C and phytic acid composition.
Containing mass volume ratio it is 0.05-0.5% in the extracting solution of the step 3 as the preferred embodiment of embodiment
Vitamin C.
As the preferred embodiment of embodiment, the plant that volume ratio is 0.01-0.1% is contained in the extracting solution of the step 3
Acid.
Containing mass volume ratio it is 0.05-0.1% in the extracting solution of the step 3 as the preferred embodiment of embodiment
Vitamin C and the phytic acid that volume ratio is 0.01-0.05%.
As the preferred embodiment of embodiment, the seeweed polyphenol product is white powder；The recovery rate of the seeweed polyphenol
For 1.5-6.5%；Purity is 90-95%.
The present invention after the above technical solution is adopted, has the advantages that：
1. the full algae utilization of resources of the present invention achievable algal polysaccharides, seeweed polyphenol, fucoxanthine, seaweed slag, is seaweed
The core technology of processing industry active demand；
2. the present invention realizes the purifying that efficiently separates of seeweed polyphenol using solid phase extraction techniques, conventional seeweed polyphenol life is reduced
Unit operations, the simplification of flowsheet such as filtering, column chromatography purifying, concentration in production. art shorten the production time, improve product
Quality, product purity >=90 mass %；
3. the characteristics of degradation oxidizable for seeweed polyphenol of the invention, being improved in extraction process by adding protective agent
The stability of seeweed polyphenol, to improve extraction efficiency.
Description of the drawings
Fig. 1 is the process flow chart of the present invention.
Specific implementation mode
The embodiment of the present invention is described below in detail, process flow chart of the invention, as shown in Figure 1.By reference to attached drawing
The embodiment of description is exemplary, it is intended to for explaining the present invention, and is not considered as limiting the invention.In embodiment
Particular technique or condition person is not specified, according to technology or condition described in document in the art or according to product description
It carries out.Reagents or instruments used without specified manufacturer, being can be with conventional products that are commercially available.
Complex enzyme used in following embodiment is 1:The pectase and cellulase complex enzyme of 1 (w/w)；Guarantor in extracting solution
It is 0.05 mass % and 0.01 volume % phytic acid to protect agent.
Embodiment 1：Kelp prepares high-purity seeweed polyphenol
(1) it is the dry kelp 1kg of 20 mass % to take water content, is impregnated after rinsing removes the impurity such as silt with tap water and uses mashing
Machine is beaten, and obtains seaweed slurry 0.6L；It is sent into blender, and 3L deionized waters is added, stirred with 120 turns/min rotating speeds under temperature
30min；Then seaweed slurry centrifuges 5min with low speed centrifuge with the rotating speed of 1000 turns/min, collect supernatant and seaweed respectively
Slag；After seaweed slag is by above-mentioned steps and the agitated machine stirring of condition, centrifuge processing, supernatant and sea are collected respectively again
Algae-residue.Merge supernatant twice, algal polysaccharides are obtained after spray-dried；Collection obtains seaweed slag 342g, is prepared for extracting
Seeweed polyphenol.
(2) it takes above-mentioned wet kelp residue to be uniformly mixed with 1.71g complex enzymes, hydrolyzes 5h at room temperature, realize that alginic cell wall is broken
Wall.
(3) seeweed polyphenol protective agent is dissolved in deionized water, is then 1 by volume with food-grade anhydrous ethyl alcohol：4
(v:V) it mixes, and acetic acid is added by volume, make the final concentration of 0.1% (v of acetic acid:V), it is the extraction of seeweed polyphenol after mixing
Liquid contains 0.05 mass % and 0.01 volume % phytic acid in extracting solution.1.71L extracting solutions are added to the seaweed slag of above-mentioned enzymolysis broken wall
In and mixing, extract 1.5h at room temperature；Then 5min is centrifuged with the rotating speed of 3000 turns/min, collects supernatant and seaweed respectively
Slag.Seaweed slag continues to carry out second extraction with above-mentioned extracting solution repetition abovementioned steps, collects supernatant and seaweed slag respectively.Seaweed
Slag is used for raw materials of feed additives after drying；Merge supernatant 3.2L twice, for isolating and purifying for seeweed polyphenol.
(4) above-mentioned supernatant is poured into the adsorption tank equipped with silica gel, liquid level is made to be flushed with silica gel, carry out Static Adsorption decoloration
2h, the pigment of silica gel absorption can be further used for preparing fucoxanthine isoreactivity substance；Then use vacuum concentration method at 40 DEG C
It is lower seeweed polyphenol extracting solution is concentrated into 1.6L volumes after, by concentrate pour into equipped with domestic XDA-7 macropores absorb resin suction
Attached pond, makes liquid level be flushed with macroreticular resin, and Solid Phase Extraction 2h is carried out to seeweed polyphenol；Macroreticular resin is pulled out with strainer, is spent
Ionized water short rinse, except impurity such as desaccharification, small peptides；Then macroreticular resin is put into the desorption equipped with food-grade anhydrous ethyl alcohol
Pond makes ethyl alcohol liquid level be flushed with macroreticular resin, impregnates 0.5h, so that the seeweed polyphenol being adsorbed on macroreticular resin is eluted and be dissolved in
In ethyl alcohol.The macroreticular resin of desorption is used further to the absorption of seeweed polyphenol next time after deionized water rinses；In desorption cell
Ethyl alcohol can multiple Reusability, with achieve the purpose that be enriched with seeweed polyphenol.
(5) ethanol solution of above-mentioned desorption is concentrated to dryness at 40 DEG C, then dry in 50 DEG C using vacuum drying
Dry 2h, obtains high-purity seeweed polyphenol powder 18.4g, and product total phenol content is 91.5 mass %.
Embodiment 2：Undaria pinnitafida prepares high-purity seeweed polyphenol
(1) it is the dry undaria pinnitafida 1kg of 20 mass % to take water content, is impregnated, rinsing, is beaten with tap water, obtains seaweed slurry
0.55L；Be sent into blender after be added 2.75L deionized waters, temperature under with 120 turns/min rotating speeds stir 30min；Then with 1000
Turn/min centrifugation 5min, collects supernatant and seaweed slag respectively；It repeats the above steps, supernatant is used to prepare algal polysaccharides；It receives
Collection obtains seaweed slag 313g, and seeweed polyphenol is prepared for extraction.
(2) it takes above-mentioned wet opotism dish slag to be uniformly mixed with 1.565g complex enzymes, hydrolyzes 5h at room temperature, realize alginic cell wall
Broken wall.
(3) using the 80 volume % ethanol waters containing 0.05 mass %, 0.01 volume % phytic acid and 0.1 volume % acetic acid
For extracting solution.1.565L extracting solutions are added in the seaweed slag of above-mentioned enzymolysis broken wall and mixing, extract 1.5h at room temperature；With 3000
Turn/min centrifugation 5min, collects supernatant and seaweed slag respectively.It repeats abovementioned steps and carries out second extraction.Seaweed slag is after drying
For raw materials of feed additives；Merge supernatant 3.0L twice, for isolating and purifying for seeweed polyphenol.
(4) above-mentioned supernatant is poured into the decoloration of the adsorption tank equipped with silica gel 2h；Supernatant is concentrated under reduced pressure at 40 DEG C
After 1.5L volumes, absorbs resin solid phase with domestic XDA-7 macropores and extract 2h；After macroreticular resin deionized water short rinse, use
Food-grade anhydrous ethyl alcohol desorption obtains the ethanol solution rich in seeweed polyphenol.
(5) ethanol solution of above-mentioned desorption is concentrated to dryness at 40 DEG C, then dry in 50 DEG C using vacuum drying
Dry 2h, obtains high-purity seeweed polyphenol powder 27.6g, and product total phenol content is 93.2 mass %.
Embodiment 3：Sargassum kjellmanianum Yendo prepares high-purity seeweed polyphenol
(1) it is the dry sargassum kjellmanianum Yendo 1kg of 20 mass % to take water content, is impregnated, rinsing, is beaten with tap water, obtains seaweed slurry
0.5L；Be sent into blender after be added 2.5L deionized waters, temperature under with 120 turns/min rotating speeds stir 30min；Then with 1000 turns/
Min centrifuges 5min, collects supernatant and seaweed slag respectively；It repeats the above steps, supernatant is used to prepare algal polysaccharides；It collects
To seaweed slag 410g, seeweed polyphenol is prepared for extraction.
(2) it takes above-mentioned wet opotism dish slag to be uniformly mixed with 2.05g complex enzymes, hydrolyzes 5h at room temperature, realize alginic cell wall
Broken wall.
(3) using the 80 volume % ethanol waters containing 0.05 mass %, 0.01 volume % phytic acid and 0.1 volume % acetic acid
For extracting solution.2.05L extracting solutions are added in the seaweed slag of above-mentioned enzymolysis broken wall and mixing, extract 1.5h at room temperature；With 3000
Turn/min centrifugation 5min, collects supernatant and seaweed slag respectively.It repeats abovementioned steps and carries out second extraction.Seaweed slag is after drying
For raw materials of feed additives；Merge supernatant 3.8L twice, for isolating and purifying for seeweed polyphenol.
(4) above-mentioned supernatant is poured into the decoloration of the adsorption tank equipped with silica gel 2h；Supernatant is concentrated under reduced pressure at 40 DEG C
After 1.9L volumes, absorbs resin solid phase with domestic XDA-7 macropores and extract 2h；After macroreticular resin deionized water short rinse, use
Food-grade anhydrous ethyl alcohol desorption obtains the ethanol solution rich in seeweed polyphenol.
(5) ethanol solution of above-mentioned desorption is concentrated to dryness at 40 DEG C, then dry in 50 DEG C using vacuum drying
Dry 2h, obtains high-purity seeweed polyphenol powder 38.5g, and product total phenol content is 90 mass %.
Embodiment 4：Sargassum fusifome prepares high-purity seeweed polyphenol
(1) it is the dry sargassum fusifome 1kg of 20 mass % to take water content, is impregnated, rinsing, is beaten with tap water, obtains seaweed slurry
0.65L；Be sent into blender after be added 3.25L deionized waters, temperature under with 120 turns/min rotating speeds stir 30min；Then with 1000
Turn/min centrifugation 5min, collects supernatant and seaweed slag respectively；It repeats the above steps, supernatant is used to prepare algal polysaccharides；It receives
Collection obtains seaweed slag 350g, and seeweed polyphenol is prepared for extraction.
(2) it takes above-mentioned wet opotism dish slag to be uniformly mixed with 1.75g complex enzymes, hydrolyzes 5h at room temperature, realize alginic cell wall
Broken wall.
(3) using the 80 volume % ethanol waters containing 0.05 mass %, 0.01 volume % phytic acid and 0.1 volume % acetic acid
For extracting solution.1.75L extracting solutions are added in the seaweed slag of above-mentioned enzymolysis broken wall and mixing, extract 1.5h at room temperature；With 3000
Turn/min centrifugation 5min, collects supernatant and seaweed slag respectively.It repeats abovementioned steps and carries out second extraction.Seaweed slag is after drying
For raw materials of feed additives；Merge supernatant 3.4L twice, for isolating and purifying for seeweed polyphenol.
(4) above-mentioned supernatant is poured into the decoloration of the adsorption tank equipped with silica gel 2h；Supernatant is concentrated under reduced pressure at 40 DEG C
After 1.7L volumes, absorbs resin solid phase with domestic XDA-7 macropores and extract 2h；After macroreticular resin deionized water short rinse, use
Food-grade anhydrous ethyl alcohol desorption obtains the ethanol solution rich in seeweed polyphenol.
(5) ethanol solution of above-mentioned desorption is concentrated to dryness at 40 DEG C, then dry in 50 DEG C using vacuum drying
Dry 2h, obtains high-purity seeweed polyphenol powder 15.3g, and product total phenol content is 94.1 mass %.
Embodiment 5：Gan Tai prepares high-purity seeweed polyphenol
(1) it is that 20 mass % do sweet tongue 1kg to take water content, is impregnated, rinsing, is beaten with tap water, obtains seaweed slurry 0.8L；
Be sent into blender after be added 4.0L deionized waters, temperature under with 120 turns/min rotating speeds stir 30min；Then with 1000 turns/min from
Heart 5min collects supernatant and seaweed slag respectively；It repeats the above steps, supernatant is used to prepare algal polysaccharides；Collection obtains sea
Algae-residue 280g prepares seeweed polyphenol for extraction.
(2) it takes above-mentioned wet opotism dish slag to be uniformly mixed with 1.4g complex enzymes, hydrolyzes 5h at room temperature, realize that alginic cell wall is broken
Wall.
(3) using the 80 volume % ethanol waters containing 0.05 mass %, 0.01 volume % phytic acid and 0.1 volume % acetic acid
For extracting solution.1.4L extracting solutions are added in the seaweed slag of above-mentioned enzymolysis broken wall and mixing, extract 1.5h at room temperature；With 3000
Turn/min centrifugation 5min, collects supernatant and seaweed slag respectively.It repeats abovementioned steps and carries out second extraction.Seaweed slag is after drying
For raw materials of feed additives；Merge supernatant 2.5L twice, for isolating and purifying for seeweed polyphenol.
(4) above-mentioned supernatant is poured into the decoloration of the adsorption tank equipped with silica gel 2h；Supernatant is concentrated under reduced pressure at 40 DEG C
After 1.25L volumes, absorbs resin solid phase with domestic XDA-7 macropores and extract 2h；After macroreticular resin deionized water short rinse, use
Food-grade anhydrous ethyl alcohol desorption obtains the ethanol solution rich in seeweed polyphenol.
(5) ethanol solution of above-mentioned desorption is concentrated to dryness at 40 DEG C, then dry in 50 DEG C using vacuum drying
Dry 2h, obtains high-purity seeweed polyphenol powder 65.2g, and product total phenol content is 95 mass %.
The characteristics of present invention is for seeweed polyphenol oxidizable degradation, sea is improved in extraction process by adding protective agent
The stability of algae polyphenol, to improve extraction efficiency.Experiment to vitamin C, is planted using the kelp residue after digesting broken wall as raw material
The protecting effect of the compound formulation of acid and its composition has carried out comparative study.Kelp residue (contains the 80% of 0.1% acetic acid with extracting solution
Ethanol water) it is fixed than being 1:5(w：V), 1.5h is extracted at room temperature, and extraction judges to protect twice, with seeweed polyphenol recovery rate
The effect of agent is protected, the results are shown in Table 1.Experimental result finds that under the action of protective agent, the recovery rate of seeweed polyphenol significantly carries
It is high.Wherein, the protecting effect of phytic acid is better than vitamin C, the complexing agent best results being made of the two.By comparing vitamin
C combines the protective effect to seeweed polyphenol with the various concentration of phytic acid, finds the guarantor of 0.05 mass % and 0.01 volume % phytic acid
Shield effect is combined with other to be not significantly different.
Influence of 1 protective agent of table to seeweed polyphenol recovery rate
In short, the present invention is based on the full algae utilization of resources to seaweed, production process is reduced to seaweed by adding protective agent
The destruction of polyphenol prepares the high efficiency of seeweed polyphenol, high-purity mesh using biological enzyme broken wall-Solid Phase Extraction joint technology realization
Mark reduces the unit operations such as the column chromatography in traditional handicraft, has the technical advantages such as environmentally protective, low energy is efficient.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case of can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (7)
1. a kind of preparation method of high-purity seeweed polyphenol, it is characterised in that：Include the following steps：
Step 1: the separation of algal polysaccharides and seaweed slag：The dry seaweed that water content is 20% is impregnated with tap water first, is rinsed
It is beaten with beater after removing silt impurity；Seaweed slurry is sent into blender, and is starched by seaweed：Deionized water volume ratio is 1：5
Deionized water is added, is stirred 30 minutes with 120 turns/min rotating speeds at room temperature；Seaweed slurry low speed centrifuge is with 1000 turns/min's
Rotating speed centrifuges 5min, collects supernatant and seaweed slag respectively；Seaweed slag is by above-mentioned steps and the agitated machine stirring of condition, centrifuge
After centrifugal treating, supernatant and seaweed slag are collected respectively again；Merge supernatant twice, it is more to obtain seaweed after spray-dried
Sugar；Seaweed slag is collected, seeweed polyphenol is prepared for extraction；
Step 2: the enzymolysis broken wall of seaweed slag：It will be by cellulase and pectase by weight 1：The complex enzyme of 1 composition is by weight
Than being 1:1000 are added in the seaweed slag, hydrolyze 5h at room temperature, realize alginic cell wall broken wall；
Step 3: the high efficiency extraction of seeweed polyphenol：Seeweed polyphenol protective agent is dissolved in deionized water, then with food-grade without
Water-ethanol is 1 by volume：4 mixing, and acetic acid is added by volume, make acetic acid final volume a concentration of 0.1%, is sea after mixing
The extracting solution of algae polyphenol；The extracting solution is 5 by volume/weight ratio with seaweed slag:1 carries out mixing, extracts 1.5h at room temperature, with
The rotating speed of 3000 turns/min centrifuges 5min, collects supernatant and seaweed slag respectively；Seaweed slag continues before being repeated with the extracting solution
It states step and carries out second extraction, collect supernatant and seaweed slag respectively；Seaweed slag is used for raw materials of feed additives after drying；It closes
And supernatant twice, for isolating and purifying for seeweed polyphenol；
Step 4: seeweed polyphenol isolates and purifies：It is quiet that supernatant made from step 3 is poured into the progress of the adsorption tank containing silica gel
State adsorption bleaching 2h, the pigment of silica gel absorption are further used for preparing fucoxanthine active material；Then vacuum concentration method is used
After seeweed polyphenol extracting solution is concentrated into 50% volume at 40 DEG C, resin is absorbed to seeweed polyphenol using domestic XDA-7 macropores
Carry out Solid Phase Extraction 2h；By XDA-7 macroreticular resins deionized water short rinse, except desaccharification, small peptide impurity；Then by XDA-7
Macroreticular resin impregnates 0.5h with food-grade anhydrous ethyl alcohol, and the seeweed polyphenol being adsorbed on macroreticular resin is eluted and is dissolved in ethyl alcohol
In, obtain ethyl alcohol soak；
Step 5: the preparation of seeweed polyphenol：The ethyl alcohol soak is concentrated to dryness at 40 DEG C, vacuum is dry at 50 DEG C
Dry 2h obtains seeweed polyphenol product.
2. a kind of preparation method of high-purity seeweed polyphenol as described in claim 1, it is characterised in that：The seaweed is sea
At least one of the sacrificial dish of band, undaria pinnitafida, sheep, sargassum kjellmanianum Yendo, sargassum thunbergii and Gan Tai.
3. a kind of preparation method of high-purity seeweed polyphenol as described in claim 1, it is characterised in that：The sea of the step 3
Algae protected polyphenol agent is vitamin C or phytic acid or the compound being made of vitamin C and phytic acid.
4. a kind of preparation method of high-purity seeweed polyphenol as described in claim 1, it is characterised in that：The step 3 carries
It takes in liquid containing the vitamin C that mass volume ratio is 0.05-0.5%.
5. a kind of preparation method of high-purity seeweed polyphenol as described in claim 1, it is characterised in that：The step 3 carries
It takes in liquid containing the phytic acid that volume ratio is 0.01-0.1%.
6. a kind of preparation method of high-purity seeweed polyphenol as described in claim 1, it is characterised in that：The step 3 carries
Take the phytic acid that the vitamin C and volume ratio that are 0.05-0.1% containing mass volume ratio in liquid are 0.01-0.05%.
7. a kind of preparation method of high-purity seeweed polyphenol as described in claim 1, it is characterised in that：The seeweed polyphenol production
Product are white powder；The recovery rate of the seeweed polyphenol is 1.5-6.5%；Purity is 90-95%.
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| CN201510648035.0A CN105193863B (en) | 2015-10-09 | 2015-10-09 | A kind of preparation method of high-purity seeweed polyphenol |
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| CN106617060A (en) * | 2016-12-27 | 2017-05-10 | 云南中烟工业有限责任公司 | Fructus phyllanthi polyphenols enriching and purifying method |
| CN114191455A (en) * | 2017-02-08 | 2022-03-18 | 中英阿诺康（宁夏）生物科技有限公司 | Extraction process and preparation method of seaweed polyphenol |
| CN107468719B (en) * | 2017-07-14 | 2020-11-20 | 大连工业大学 | High-efficiency extraction method of algae polyphenol |
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| CN111978435B (en) * | 2019-05-22 | 2021-05-25 | 合肥博思科创医药科技有限公司 | Preparation method of high-purity sugammadex sodium |
| CN111000875A (en) * | 2019-11-18 | 2020-04-14 | 青岛科技大学 | Extraction method of kelp polyphenol |
| CN110755459B (en) * | 2019-11-22 | 2021-06-29 | 广西南亚热带农业科学研究所 | Extraction process of annona squamosa leaf polyphenol |
| CN112472726A (en) * | 2021-01-07 | 2021-03-12 | 山东洁晶集团股份有限公司 | Extraction method of brown algae polyphenol stock solution |
| CN115337329A (en) * | 2022-08-24 | 2022-11-15 | 中国海洋大学 | Preparation method of sargassum thunbergii polyphenol |
| TWI828313B (en) * | 2022-09-13 | 2024-01-01 | 誠光生物科技股份有限公司 | Method for preparing algae polysaccharide extract |
| CN115645312B (en) * | 2022-10-11 | 2023-12-12 | 江苏海洋大学 | Application of sargassum pallidum polyphenol in preparing whitening cosmetics and preparation method thereof |
| CN117137955A (en) * | 2023-08-24 | 2023-12-01 | 中国海洋大学 | Seaweed polyphenol and preparation method and application thereof |
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