CN105193863A - Preparation method of high-purity algal polyphenol - Google Patents
Preparation method of high-purity algal polyphenol Download PDFInfo
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Abstract
The invention discloses a preparation method of high-purity algal polyphenol. The preparation method comprises the process steps of separation of algal polysaccharide and alga residues, enzymolysis wall breaking of the alga residues, efficient extraction of algal polyphenol, separation and purification of the algal polyphenol, and obtaining of the high-purity algal polyphenol. According to the preparation method, full-alga comprehensive utilization of the algal polysaccharide, the algal polyphenol and the alga residues is realized.
Description
Technical field
The present invention relates to the technical field of seeweed polyphenol, particularly relate to a kind of preparation method of high-purity seeweed polyphenol.
Background technology
Sargassum is the main source of sea-plant polyphenol, and its structure and Lu Yuan plant polyphenol exist a great difference: Lu Yuan plant polyphenol is derived by gallic acid and flower acid of mixing; Seeweed polyphenol is then the derivant of phloroglucinol.Research display, seeweed polyphenol at antioxidation, improve in metabolic syndrome, control degenerative disease etc. and have specially good effect, and safety non-toxic.Therefore, American-European countries drops into the Application and Development that huge fund implements seeweed polyphenol in succession.High-purity seeweed polyphenol has the advantages such as biological activity is strong, medical value is high, good stability, is the product of biomedicine field urgent needs.
But because seeweed polyphenol is present in the algae bubble of alginic cell inside, embedded by algin, cellulose even depth, conventional extraction techniques is difficult to obtain high yield, and production cost is high, and purity is lower.Such as, Chinese invention patent application CN102579508A " a kind of preparation method of Sargassum fusiforme (Harv.) Setch brown algae polyphenols ", open is raw material with Sargassum fusiforme (Harv.) Setch, adopts methanol heating extraction (40 DEG C), then adopts different solvents extraction and ultrafiltration to retain means and prepares brown algae polyphenols; Chinese invention patent application CN102397300A " a kind of extracting method of brown algae polyphenols ", disclose with Fresh Laminaria Japonica, sargassum thunbergii, Thallus Sargassi Kjellmaniani as raw material, the solvent extraction of employing machine, purification by macroporous resin prepare 3 kinds of brown algae polyphenols, and its productive rate is respectively 0.3 ‰, 2.5 ‰, 3 ‰; Chinese invention patent application CN103610704A " a kind of extracting method of brown algae polyphenols ", open with fresh Sargassum Brown algae or Thallus Laminariae (Thallus Eckloniae) for raw material, organic solvent lixiviate in hot bath is adopted after broken, after purification by macroporous resin, eluting, concentrated, lyophilization, obtain brown algae polyphenols extract, productive rate is 2.5 ‰; Chinese invention patent application CN104382951A " a kind of extracting method of seeweed polyphenol ", disclose with Chlorella pyrenoidesa, Euglena, salt alga three kinds of algae as raw material, take ethanol as solvent, adopt microwave combined extractive technique, after extracting liquid filtering, obtain the polyphenol extract of 3 kinds of Sargassums through lyophilization; Chinese invention patent mandate CN102935093B " a kind of extracting method of seeweed polyphenol ", discloses with 40 object Sargassum powder for raw material, adopts microwave-assisted water extraction to extract, then obtains the polyphenol extract of purity about 75% through purification by macroporous resin; Chinese invention patent mandate CN102166230B " method of microwave-assisted seeweed polyphenol ", open is raw material with Sargassum powder, with alcohol-acetone-water mixed solvent, extracts seeweed polyphenol in conjunction with microwave technology, after filtration, lyophilization obtains seeweed polyphenol crude extract, and extraction ratio can reach 2.26%.The above-mentioned method preparing seeweed polyphenol lacks the comprehensive utilization to main components such as Algins, serious waste of resources; Also there is following problem in the above-mentioned Technology preparing seeweed polyphenol simultaneously: 1) inferior separating effect, purity is low.Seeweed polyphenol easily and alginate jelly, albumen form complex with the form of non-covalent bond, be difficult to be isolated in follow-up purge process, cause the response rate of seeweed polyphenol low; In addition, also containing a large amount of fat-soluble pigment in the seeweed polyphenol of extraction, conventional post chromatographic technique cannot realize effective separation, causes the purity of product low.2) structural deterioration is large, active low.Seeweed polyphenol extremely unstable, oxidizable, the high temperature in the course of processing, alkaline ph values, oxygen etc. all can destroy its biological activity.Although microwave technology, ultrasound-assisted extraction technology can improve the yield of Sargassum ocean polyphenol, leaching process can produce high temperature, adds shortage effective protection measure, accelerates the oxidation of ocean polyphenol under the effect of the oxygen, causes loss of activity.3) complex manufacturing, cost is high.At present comprise pulverizing, extraction, centrifugal, filtration, upper prop, eluting, resin regeneration, the repeatedly multiple working procedure such as concentrated, dry for the technique of processing seeweed polyphenol; Conventional column chromatography purification seeweed polyphenol also must be equipped with the equipment such as constant flow pump, glass column, gathering-device, and cause the production time long, equipment requirements is high, limits industrialized development.This is the key technology bottleneck causing seeweed polyphenol commercial application.
In view of this, the present inventor studies and devises a kind of preparation method of high-purity seeweed polyphenol, and this case produces thus.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high-purity seeweed polyphenol, comprise being separated of Sargassum polysaccharides and Sargassum slag, the enzymolysis breaking cellular wall of Sargassum slag, the processing step such as high efficiency extraction, the separation and purification of seeweed polyphenol, the acquisition of high-purity seeweed polyphenol of seeweed polyphenol, to realize the full algae comprehensive utilization of Sargassum polysaccharides, seeweed polyphenol, Sargassum slag.
To achieve these goals, the present invention solves the technical scheme that its technical problem takes and is:
A preparation method for high-purity seeweed polyphenol, comprises the following steps:
Step one, Sargassum polysaccharides are separated with Sargassum slag: first by water content be 20% dry seaweed tap water soak, rinsing removing silt impurity after pull an oar with beater; Sargassum slurry is sent in blender, and starches by Sargassum: deionized water volume ratio is that 1:5 adds deionized water, stirs 30 minutes under room temperature with 120 turns/min rotating speed; Sargassum slurry low speed centrifuge, with the centrifugal 5min of the rotating speed of 1000 turns/min, collects supernatant and Sargassum slag respectively; Sargassum slag stirs through blender by above-mentioned steps and condition, after centrifuge process, again collect supernatant and Sargassum slag respectively; Merge twice supernatant, after spray-dried, obtain Sargassum polysaccharides; Collecting Sargassum slag, preparing seeweed polyphenol for extracting;
The enzymolysis breaking cellular wall of step 2, Sargassum slag: the compound enzyme be made up of by weight 1:1 cellulase and pectase is joined in described Sargassum slag by weight for 1:1000, is hydrolyzed 5h under room temperature, realizes alginic cell wall breaking cellular wall;
The high efficiency extraction of step 3, seeweed polyphenol: seeweed polyphenol protective agent is dissolved in deionized water, then with food-grade anhydrous ethanol by volume for 1:4 mixes, and add acetic acid by volume, making acetic acid final volume concentration be 0.1%, is the extracting solution of seeweed polyphenol after mixing; Described extracting solution and Sargassum slag by volume/weight ratio is that 5:1 mixes, and extracts 1.5h under room temperature, with the centrifugal 5min of the rotating speed of 3000 turns/min, collects supernatant and Sargassum slag respectively; Sargassum slag continues to repeat abovementioned steps with described extracting solution and carries out second extraction, collects supernatant and Sargassum slag respectively; Sargassum slag is after drying for raw materials of feed additives; Merge twice supernatant, for the separation and purification of seeweed polyphenol;
The separation and purification of step 4, seeweed polyphenol: supernatant step 3 the obtained adsorption tank poured into containing silica gel carries out static adsorption decolouring 2h, and the pigment of silica gel adsorption is further used for preparing fucoxanthine active substance; Then, after adopting concentrating under reduced pressure method, at 40 DEG C, seeweed polyphenol extracting solution is concentrated into 50% volume, adopt domestic XDA-7 macropore to absorb resin and Solid-Phase Extraction 2h is carried out to seeweed polyphenol; By XDA-7 macroporous resin deionized water short rinse, except desaccharide, little peptide impurity; Then by the food-grade anhydrous soak with ethanol 0.5h of XDA-7 macroporous resin, will the seeweed polyphenol eluting on macroporous resin be adsorbed in and be dissolved in ethanol, obtain soak with ethanol liquid;
The preparation of step 5, seeweed polyphenol: be evaporated to dry at 40 DEG C by described soak with ethanol liquid, vacuum drying 2h at 50 DEG C, obtains seeweed polyphenol product.
As the optimal way of embodiment, described Sargassum is at least one in Thallus Laminariae (Thallus Eckloniae), Thallus Laminariae, the sacrificial dish of sheep, Thallus Sargassi Kjellmaniani, sargassum thunbergii and Gan Tai.
As the optimal way of embodiment, the complex that the seeweed polyphenol protective agent of described step 3 is vitamin C or phytic acid or is made up of vitamin C and phytic acid.
As the optimal way of embodiment, containing mass volume ratio in the extracting solution of described step 3 is the vitamin C of 0.05-0.5%.
As the optimal way of embodiment, containing volume ratio in the extracting solution of described step 3 is the phytic acid of 0.01-0.1%.
As the optimal way of embodiment, be the vitamin C of 0.05-0.1% and volume ratio containing mass volume ratio in the extracting solution of described step 3 be the phytic acid of 0.01-0.05%.
As the optimal way of embodiment, described seeweed polyphenol product is white powder; The extraction ratio of described seeweed polyphenol is 1.5-6.5%; Purity is 90-95%.
After the present invention adopts above technical scheme, there is following beneficial effect:
1. the present invention can realize the full algae utilization of resources of Sargassum polysaccharides, seeweed polyphenol, fucoxanthine, Sargassum slag, is the core technology of Sargassum processing industry urgent needs;
2. the present invention adopts solid phase extraction techniques to realize the high efficiency separation purification of seeweed polyphenol, reduce the filtration in conventional seeweed polyphenol production technology, column chromatography purification, the unit operations such as concentrated, simplification of flowsheet, shortens the production time, improve product quality, product purity all >=90 quality %;
3. the present invention is directed to the feature of the oxidizable degraded of seeweed polyphenol, in leaching process, improve the stability of seeweed polyphenol by adding protective agent, thus improve extraction efficiency.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention.
Detailed description of the invention
Embodiments of the invention are described below in detail, process chart of the present invention, as shown in Figure 1.The embodiment described by reference to accompanying drawing is exemplary, is intended to for explaining the present invention, and can not be interpreted as limitation of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by the conventional products of commercial acquisition.
Following examples compound enzyme used is pectase and the cellulase compound enzyme of 1:1 (w/w); Protective agent in extracting solution is 0.05 quality % and 0.01 volume % phytic acid.
Embodiment 1: Thallus Laminariae (Thallus Eckloniae) prepares high-purity seeweed polyphenol
(1) getting water content is the dry Thallus Laminariae (Thallus Eckloniae) 1kg of 20 quality %, pulls an oar, obtain Sargassum slurry 0.6L with tap water after soaking the impurity such as rinsing removing silt with beater; Send in agitator, and add 3L deionized water, under temperature, stir 30min with 120 turns/min rotating speed; Then Sargassum slurry uses low speed centrifuge with the centrifugal 5min of the rotating speed of 1000 turns/min, collects supernatant and Sargassum slag respectively; Sargassum slag stirs through blender by above-mentioned steps and condition, after centrifuge process, again collect supernatant and Sargassum slag respectively.Merge twice supernatant, after spray-dried, obtain Sargassum polysaccharides; Collection obtains Sargassum slag 342g, prepares seeweed polyphenol for extracting.
(2) get above-mentioned wet kelp residue to mix homogeneously with 1.71g compound enzyme, under room temperature, be hydrolyzed 5h, realize alginic cell wall breaking cellular wall.
(3) seeweed polyphenol protective agent is dissolved in deionized water; then mix for 1:4 (v:v) by volume with food-grade anhydrous ethanol; and add acetic acid by volume; acetic acid final concentration is made to be 0.1% (v:v); be the extracting solution of seeweed polyphenol after mixing, containing 0.05 quality % and 0.01 volume % phytic acid in extracting solution.1.71L extracting solution to join in the Sargassum slag of above-mentioned enzymolysis breaking cellular wall and mixes, and extracts 1.5h under room temperature; Then with the centrifugal 5min of the rotating speed of 3000 turns/min, supernatant and Sargassum slag is collected respectively.Sargassum slag continues to repeat abovementioned steps with above-mentioned extracting solution and carries out second extraction, collects supernatant and Sargassum slag respectively.Sargassum slag is after drying for raw materials of feed additives; Merge twice supernatant 3.2L, for the separation and purification of seeweed polyphenol.
(4) above-mentioned supernatant is poured into the adsorption tank that silica gel is housed, liquid level is flushed with silica gel, carry out static adsorption decolouring 2h, the pigment of silica gel adsorption can be further used for preparing fucoxanthine isoreactivity material; Then, after adopting concentrating under reduced pressure method, at 40 DEG C, seeweed polyphenol extracting solution is concentrated into 1.6L volume, concentrated solution is poured into the adsorption tank that domestic XDA-7 macropore absorbs resin is housed, liquid level is flushed with macroporous resin, Solid-Phase Extraction 2h is carried out to seeweed polyphenol; With filter screen, macroporous resin is pulled out, use deionized water short rinse, except the impurity such as desaccharide, little peptide; Then macroporous resin is put into the desorption cell that food-grade anhydrous ethanol is housed, ethanol liquid level is flushed with macroporous resin, soak 0.5h, make the seeweed polyphenol eluting that is adsorbed on macroporous resin and be dissolved in ethanol.The macroporous resin of desorption is used further to the absorption of seeweed polyphenol next time after rinsed with deionized water; In desorption cell, ethanol can repeatedly Reusability, to reach the object of enrichment seeweed polyphenol.
(5) alcoholic solution of above-mentioned desorption is evaporated to dry at 40 DEG C, and then adopt vacuum drying in 50 DEG C of dry 2h, obtain high-purity seeweed polyphenol powder 18.4g, product total phenol content is 91.5 quality %.
Embodiment 2: Thallus Laminariae prepares high-purity seeweed polyphenol
(1) getting water content is the dry Thallus Laminariae 1kg of 20 quality %, with tap water immersion, rinsing, making beating, obtains Sargassum slurry 0.55L; Add 2.75L deionized water after sending into agitator, under temperature, stir 30min with 120 turns/min rotating speed; Then with the centrifugal 5min of 1000 turns/min, supernatant and Sargassum slag is collected respectively; Repeat above-mentioned steps, supernatant is for the preparation of Sargassum polysaccharides; Collection obtains Sargassum slag 313g, prepares seeweed polyphenol for extracting.
(2) get above-mentioned wet Thallus Laminariae slag to mix homogeneously with 1.565g compound enzyme, be hydrolyzed 5h under room temperature, realize alginic cell wall breaking cellular wall.
(3) the 80 volume % ethanol waters containing 0.05 quality %, 0.01 volume % phytic acid and 0.1 volume % acetic acid are adopted to be extracting solution.1.565L extracting solution to join in the Sargassum slag of above-mentioned enzymolysis breaking cellular wall and mixes, and extracts 1.5h under room temperature; With the centrifugal 5min of 3000 turns/min, collect supernatant and Sargassum slag respectively.Repeat abovementioned steps and carry out second extraction.Sargassum slag is after drying for raw materials of feed additives; Merge twice supernatant 3.0L, for the separation and purification of seeweed polyphenol.
(4) above-mentioned supernatant is poured into the adsorption tank decolouring 2h that silica gel is housed; After supernatant being evaporated to 1.5L volume at 40 DEG C, absorb resin solid phase extraction 2h with domestic XDA-7 macropore; Macroporous resin, with after deionized water short rinse, adsorbs with food-grade anhydrous ethanolysis, obtains the alcoholic solution being rich in seeweed polyphenol.
(5) alcoholic solution of above-mentioned desorption is evaporated to dry at 40 DEG C, and then adopt vacuum drying in 50 DEG C of dry 2h, obtain high-purity seeweed polyphenol powder 27.6g, product total phenol content is 93.2 quality %.
Embodiment 3: Thallus Sargassi Kjellmaniani prepares high-purity seeweed polyphenol
(1) getting water content is the dry Thallus Sargassi Kjellmaniani 1kg of 20 quality %, with tap water immersion, rinsing, making beating, obtains Sargassum slurry 0.5L; Add 2.5L deionized water after sending into agitator, under temperature, stir 30min with 120 turns/min rotating speed; Then with the centrifugal 5min of 1000 turns/min, supernatant and Sargassum slag is collected respectively; Repeat above-mentioned steps, supernatant is for the preparation of Sargassum polysaccharides; Collection obtains Sargassum slag 410g, prepares seeweed polyphenol for extracting.
(2) get above-mentioned wet Thallus Laminariae slag to mix homogeneously with 2.05g compound enzyme, be hydrolyzed 5h under room temperature, realize alginic cell wall breaking cellular wall.
(3) the 80 volume % ethanol waters containing 0.05 quality %, 0.01 volume % phytic acid and 0.1 volume % acetic acid are adopted to be extracting solution.2.05L extracting solution to join in the Sargassum slag of above-mentioned enzymolysis breaking cellular wall and mixes, and extracts 1.5h under room temperature; With the centrifugal 5min of 3000 turns/min, collect supernatant and Sargassum slag respectively.Repeat abovementioned steps and carry out second extraction.Sargassum slag is after drying for raw materials of feed additives; Merge twice supernatant 3.8L, for the separation and purification of seeweed polyphenol.
(4) above-mentioned supernatant is poured into the adsorption tank decolouring 2h that silica gel is housed; After supernatant being evaporated to 1.9L volume at 40 DEG C, absorb resin solid phase extraction 2h with domestic XDA-7 macropore; Macroporous resin, with after deionized water short rinse, adsorbs with food-grade anhydrous ethanolysis, obtains the alcoholic solution being rich in seeweed polyphenol.
(5) alcoholic solution of above-mentioned desorption is evaporated to dry at 40 DEG C, and then adopt vacuum drying in 50 DEG C of dry 2h, obtain high-purity seeweed polyphenol powder 38.5g, product total phenol content is 90 quality %.
Embodiment 4: Sargassum fusiforme (Harv.) Setch prepares high-purity seeweed polyphenol
(1) getting water content is the dry Sargassum fusiforme (Harv.) Setch 1kg of 20 quality %, with tap water immersion, rinsing, making beating, obtains Sargassum slurry 0.65L; Add 3.25L deionized water after sending into agitator, under temperature, stir 30min with 120 turns/min rotating speed; Then with the centrifugal 5min of 1000 turns/min, supernatant and Sargassum slag is collected respectively; Repeat above-mentioned steps, supernatant is for the preparation of Sargassum polysaccharides; Collection obtains Sargassum slag 350g, prepares seeweed polyphenol for extracting.
(2) get above-mentioned wet Thallus Laminariae slag to mix homogeneously with 1.75g compound enzyme, be hydrolyzed 5h under room temperature, realize alginic cell wall breaking cellular wall.
(3) the 80 volume % ethanol waters containing 0.05 quality %, 0.01 volume % phytic acid and 0.1 volume % acetic acid are adopted to be extracting solution.1.75L extracting solution to join in the Sargassum slag of above-mentioned enzymolysis breaking cellular wall and mixes, and extracts 1.5h under room temperature; With the centrifugal 5min of 3000 turns/min, collect supernatant and Sargassum slag respectively.Repeat abovementioned steps and carry out second extraction.Sargassum slag is after drying for raw materials of feed additives; Merge twice supernatant 3.4L, for the separation and purification of seeweed polyphenol.
(4) above-mentioned supernatant is poured into the adsorption tank decolouring 2h that silica gel is housed; After supernatant being evaporated to 1.7L volume at 40 DEG C, absorb resin solid phase extraction 2h with domestic XDA-7 macropore; Macroporous resin, with after deionized water short rinse, adsorbs with food-grade anhydrous ethanolysis, obtains the alcoholic solution being rich in seeweed polyphenol.
(5) alcoholic solution of above-mentioned desorption is evaporated to dry at 40 DEG C, and then adopt vacuum drying in 50 DEG C of dry 2h, obtain high-purity seeweed polyphenol powder 15.3g, product total phenol content is 94.1 quality %.
Embodiment 5: sweet tongue prepares high-purity seeweed polyphenol
(1) getting water content is that 20 quality % do sweet tongue 1kg, with tap water immersion, rinsing, making beating, obtains Sargassum slurry 0.8L; Add 4.0L deionized water after sending into agitator, under temperature, stir 30min with 120 turns/min rotating speed; Then with the centrifugal 5min of 1000 turns/min, supernatant and Sargassum slag is collected respectively; Repeat above-mentioned steps, supernatant is for the preparation of Sargassum polysaccharides; Collection obtains Sargassum slag 280g, prepares seeweed polyphenol for extracting.
(2) get above-mentioned wet Thallus Laminariae slag to mix homogeneously with 1.4g compound enzyme, be hydrolyzed 5h under room temperature, realize alginic cell wall breaking cellular wall.
(3) the 80 volume % ethanol waters containing 0.05 quality %, 0.01 volume % phytic acid and 0.1 volume % acetic acid are adopted to be extracting solution.1.4L extracting solution to join in the Sargassum slag of above-mentioned enzymolysis breaking cellular wall and mixes, and extracts 1.5h under room temperature; With the centrifugal 5min of 3000 turns/min, collect supernatant and Sargassum slag respectively.Repeat abovementioned steps and carry out second extraction.Sargassum slag is after drying for raw materials of feed additives; Merge twice supernatant 2.5L, for the separation and purification of seeweed polyphenol.
(4) above-mentioned supernatant is poured into the adsorption tank decolouring 2h that silica gel is housed; After supernatant being evaporated to 1.25L volume at 40 DEG C, absorb resin solid phase extraction 2h with domestic XDA-7 macropore; Macroporous resin, with after deionized water short rinse, adsorbs with food-grade anhydrous ethanolysis, obtains the alcoholic solution being rich in seeweed polyphenol.
(5) alcoholic solution of above-mentioned desorption is evaporated to dry at 40 DEG C, and then adopt vacuum drying in 50 DEG C of dry 2h, obtain high-purity seeweed polyphenol powder 65.2g, product total phenol content is 95 quality %.
The present invention is directed to the feature of the oxidizable degraded of seeweed polyphenol, in leaching process, improve the stability of seeweed polyphenol by adding protective agent, thus improve extraction efficiency.Experiment for raw material, has carried out comparative study to the protected effect of the compound formulation of vitamin C, phytic acid and composition thereof with the kelp residue after enzymolysis breaking cellular wall.The fixing ratio of kelp residue and extracting solution (80% ethanol water containing 0.1% acetic acid) is 1:5 (w:v), extracts 1.5h under room temperature, and extract twice, judge protectant effect with seeweed polyphenol extraction ratio, result is as shown in table 1.Experimental result finds, under protectant effect, the extraction ratio of seeweed polyphenol significantly improves.Wherein, the protected effect of phytic acid is better than vitamin C, the complexing agent best results be made up of the two.Combine the protective effect to seeweed polyphenol by the variable concentrations comparing vitamin C and phytic acid, find the protected effect of 0.05 quality % and 0.01 volume % phytic acid and other combine and there is no significant difference.
Table 1 protective agent is on the impact of seeweed polyphenol extraction ratio
In a word; the present invention is based on the full algae utilization of resources to Sargassum; production process is reduced to the destruction of seeweed polyphenol by adding protective agent; enzyme breaking cellular wall-Solid-Phase Extraction multiple techniques is adopted to realize preparing high efficiency, the high-purity target of seeweed polyphenol; reduce the unit operationss such as the column chromatography in traditional handicraft, there is the technical advantages such as environmental protection, mental retardation is efficient.
Although illustrate and describe embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art can change above-described embodiment within the scope of the invention when not departing from principle of the present invention and aim, revising, replacing and modification.
Claims (7)
1. a preparation method for high-purity seeweed polyphenol, is characterized in that: comprise the following steps:
Step one, Sargassum polysaccharides are separated with Sargassum slag: first by water content be 20% dry seaweed tap water soak, rinsing removing silt impurity after pull an oar with beater; Sargassum slurry is sent in blender, and starches by Sargassum: deionized water volume ratio is that 1:5 adds deionized water, stirs 30 minutes under room temperature with 120 turns/min rotating speed; Sargassum slurry low speed centrifuge, with the centrifugal 5min of the rotating speed of 1000 turns/min, collects supernatant and Sargassum slag respectively; Sargassum slag stirs through blender by above-mentioned steps and condition, after centrifuge process, again collect supernatant and Sargassum slag respectively; Merge twice supernatant, after spray-dried, obtain Sargassum polysaccharides; Collecting Sargassum slag, preparing seeweed polyphenol for extracting;
The enzymolysis breaking cellular wall of step 2, Sargassum slag: the compound enzyme be made up of by weight 1:1 cellulase and pectase is joined in described Sargassum slag by weight for 1:1000, is hydrolyzed 5h under room temperature, realizes alginic cell wall breaking cellular wall;
The high efficiency extraction of step 3, seeweed polyphenol: seeweed polyphenol protective agent is dissolved in deionized water, then with food-grade anhydrous ethanol by volume for 1:4 mixes, and add acetic acid by volume, making acetic acid final volume concentration be 0.1%, is the extracting solution of seeweed polyphenol after mixing; Described extracting solution and Sargassum slag by volume/weight ratio is that 5:1 mixes, and extracts 1.5h under room temperature, with the centrifugal 5min of the rotating speed of 3000 turns/min, collects supernatant and Sargassum slag respectively; Sargassum slag continues to repeat abovementioned steps with described extracting solution and carries out second extraction, collects supernatant and Sargassum slag respectively; Sargassum slag is after drying for raw materials of feed additives; Merge twice supernatant, for the separation and purification of seeweed polyphenol;
The separation and purification of step 4, seeweed polyphenol: supernatant step 3 the obtained adsorption tank poured into containing silica gel carries out static adsorption decolouring 2h, and the pigment of silica gel adsorption is further used for preparing fucoxanthine active substance; Then, after adopting concentrating under reduced pressure method, at 40 DEG C, seeweed polyphenol extracting solution is concentrated into 50% volume, adopt domestic XDA-7 macropore to absorb resin and Solid-Phase Extraction 2h is carried out to seeweed polyphenol; By XDA-7 macroporous resin deionized water short rinse, except desaccharide, little peptide impurity; Then by the food-grade anhydrous soak with ethanol 0.5h of XDA-7 macroporous resin, will the seeweed polyphenol eluting on macroporous resin be adsorbed in and be dissolved in ethanol, obtain soak with ethanol liquid;
The preparation of step 5, seeweed polyphenol: be evaporated to dry at 40 DEG C by described soak with ethanol liquid, vacuum drying 2h at 50 DEG C, obtains seeweed polyphenol product.
2. the preparation method of a kind of high-purity seeweed polyphenol as claimed in claim 1, is characterized in that: described Sargassum is at least one in Thallus Laminariae (Thallus Eckloniae), Thallus Laminariae, the sacrificial dish of sheep, Thallus Sargassi Kjellmaniani, sargassum thunbergii and Gan Tai.
3. the preparation method of a kind of high-purity seeweed polyphenol as claimed in claim 1, is characterized in that: the complex that the seeweed polyphenol protective agent of described step 3 is vitamin C or phytic acid or is made up of vitamin C and phytic acid.
4. the preparation method of a kind of high-purity seeweed polyphenol as claimed in claim 1, is characterized in that: containing mass volume ratio in the extracting solution of described step 3 is the vitamin C of 0.05-0.5%.
5. the preparation method of a kind of high-purity seeweed polyphenol as claimed in claim 1, is characterized in that: containing volume ratio in the extracting solution of described step 3 is the phytic acid of 0.01-0.1%.
6. the preparation method of a kind of high-purity seeweed polyphenol as claimed in claim 1, is characterized in that: be the vitamin C of 0.05-0.1% and volume ratio containing mass volume ratio in the extracting solution of described step 3 be the phytic acid of 0.01-0.05%.
7. the preparation method of a kind of high-purity seeweed polyphenol as claimed in claim 1, is characterized in that: described seeweed polyphenol product is white powder; The extraction ratio of described seeweed polyphenol is 1.5-6.5%; Purity is 90-95%.
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| CN105852114A (en) * | 2016-05-07 | 2016-08-17 | 集美大学 | Lipid lowering and liver protecting functional food |
| CN105996027A (en) * | 2016-05-07 | 2016-10-12 | 集美大学 | Functional food with effects of protecting liver and improving eyesight |
| CN106619744A (en) * | 2017-02-08 | 2017-05-10 | 中英阿诺康（宁夏）生物科技有限公司 | Extraction technique and preparation method of algal polyphenols |
| 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 |
| CN107468719A (en) * | 2017-07-14 | 2017-12-15 | 大连工业大学 | A kind of algae polyphenol highly effective extraction method |
| CN108434177A (en) * | 2018-03-30 | 2018-08-24 | 中国农业科学院烟草研究所 | A kind of activity inhibitor and preparation method thereof and its in application hypoglycemic, in reducing blood lipid |
| CN109123321A (en) * | 2018-08-07 | 2019-01-04 | 河南丰之源生物科技有限公司 | A kind of extraction and preparation process of apple polyphenol |
| CN110755459A (en) * | 2019-11-22 | 2020-02-07 | 广西南亚热带农业科学研究所 | Extraction process of annona squamosa leaf polyphenol |
| CN111978435A (en) * | 2019-05-22 | 2020-11-24 | 合肥博思科创医药科技有限公司 | Preparation method of high-purity sugammadex sodium |
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| WO2021098164A1 (en) * | 2019-11-18 | 2021-05-27 | 青岛科技大学 | Method for extracting kelp polyphenols |
| CN115337329A (en) * | 2022-08-24 | 2022-11-15 | 中国海洋大学 | Preparation method of sargassum thunbergii polyphenol |
| CN115645312A (en) * | 2022-10-11 | 2023-01-31 | 江苏海洋大学 | Application of sargassum pallidum polyphenol in preparing whitening cosmetics and preparation method of sargassum pallidum polyphenol |
| CN116082087A (en) * | 2022-12-28 | 2023-05-09 | 青岛苏贝尔作物营养有限公司 | Brown algae polyphenol-iron complex for preventing and treating plant yellowing and preparation method thereof |
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| CN105852114A (en) * | 2016-05-07 | 2016-08-17 | 集美大学 | Lipid lowering and liver protecting functional food |
| CN105996027A (en) * | 2016-05-07 | 2016-10-12 | 集美大学 | Functional food with effects of protecting liver and improving eyesight |
| CN105996027B (en) * | 2016-05-07 | 2019-05-10 | 集美大学 | A kind of functional food of liver protection and eyesight |
| 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 |
| CN106619744A (en) * | 2017-02-08 | 2017-05-10 | 中英阿诺康（宁夏）生物科技有限公司 | Extraction technique and preparation method of algal polyphenols |
| 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 |
| CN107468719A (en) * | 2017-07-14 | 2017-12-15 | 大连工业大学 | A kind of algae polyphenol highly effective extraction method |
| CN107468719B (en) * | 2017-07-14 | 2020-11-20 | 大连工业大学 | High-efficiency extraction method of algae polyphenol |
| CN108434177A (en) * | 2018-03-30 | 2018-08-24 | 中国农业科学院烟草研究所 | A kind of activity inhibitor and preparation method thereof and its in application hypoglycemic, in reducing blood lipid |
| CN109123321A (en) * | 2018-08-07 | 2019-01-04 | 河南丰之源生物科技有限公司 | A kind of extraction and preparation process of apple polyphenol |
| CN111978435A (en) * | 2019-05-22 | 2020-11-24 | 合肥博思科创医药科技有限公司 | Preparation method of high-purity sugammadex sodium |
| 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 |
| US11306158B1 (en) | 2019-05-22 | 2022-04-19 | Hefei Bosikc Pharmtech Co., Ltd. | Method for preparing high-purity sugammadex sodium |
| WO2021098164A1 (en) * | 2019-11-18 | 2021-05-27 | 青岛科技大学 | Method for extracting kelp polyphenols |
| CN110755459A (en) * | 2019-11-22 | 2020-02-07 | 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 |
| CN115645312A (en) * | 2022-10-11 | 2023-01-31 | 江苏海洋大学 | Application of sargassum pallidum polyphenol in preparing whitening cosmetics and preparation method of sargassum pallidum polyphenol |
| 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 |
| CN116082087A (en) * | 2022-12-28 | 2023-05-09 | 青岛苏贝尔作物营养有限公司 | Brown algae polyphenol-iron complex for preventing and treating plant yellowing 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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