CN102336725B - Method for extracting fucoxanthine-containing concentrate, product obtained through method, and application of product - Google Patents
Method for extracting fucoxanthine-containing concentrate, product obtained through method, and application of product Download PDFInfo
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Abstract
The invention relates to a method for extracting a fucoxanthine-containing concentrate from algae, the fucoxanthine-containing concentrate obtained through the method, and application of the fucoxanthine-containing concentrate. The method comprises the following steps of: pretreating raw materials; performing enzyme treatment; extracting; separating; concentrating and the like. The method overcomes technical defects of low efficiency of extracting fucoxanthine and high consumption of an organic solvent in the prior art, and a fucoxanthine product with high active ingredients is obtained, so the fucoxanthine product has a good application prospect. The raw materials are readily available, the extraction process is simple, and the obtained product has stable content and controllable comprehensive cost, and is suitable for industrial production and lengthening an industrial chain.
Description
[technical field]
The invention belongs to from the technical field of extracted form natural plant effective constituent.More specifically, the present invention relates to a kind of method of extracting the enriched material that contains fucoxanthine from marine alga, also relate to the enriched material that contains fucoxanthine that adopts aforesaid method to obtain, the purposes of the enriched material that contains fucoxanthine described in also relating to.
[background technology]
The marine alga growing in ocean, particularly biological (comprising sea-tangle (Laminaria japonica), Sargassum fusiforme (Sargassum fusiforme), sargassun (Sargassum), bulk kelp (Macrocystis pyrifera (L.) Ag), wakame (Undaria pinnatifida), Thallus Gracilariae (Gracilaria sp) etc.) body of phaeophyta (Phaeophyta) contains abundant carotinoid compounds, wherein fucoxanthine ratio is the highest, is the natural resources of comparatively desirable extraction fucoxanthine.
Fucoxanthine, is also pheophytin, and English name is Fucoxanthin, molecular formula C
42h
58o
6, be a kind of rare containing oxygen carotenoid in phaeophyta biology of being present in, half systematic naming method be 3 '-ethanoyl-6 ', 7 '-dideoxy-5,6-epoxy group(ing)-5,5 ', 6,6 ', 7,8-, six hydrogen-3,5 '-dihydroxyl-8-carbonyl-β, β-carotene.As the one of xenthophylls, its molecule is made up of the end group of a poly alkene chain and two ring-types, in solution He under unbound state, is revealed as tawny, fucoxanthine has multiple pairs of keys, have geometrical isomer at occurring in nature, and taking alltrans as main, its structural formula is as follows.
At present, some about the report of fucoxanthine extracting method.As patent CN100999508A discloses a kind of method of extracting fucoxanthine from brown alga, the method is taking brown alga as raw material, through 60%～100% extraction using alcohol, concentrated, filtering-depositing, macroporous adsorbent resin column chromatography, the dry product that makes of spraying, measure through HPLC method, in this product, the weight content of fucoxanthine is 1%～20%.But present method exists extraction time long, the defect such as complex process, extracts yield lower, and impurity is many.If can, before extracting, carry out broken wall treatment to raw material, contribute to the release of target product, can shorten greatly extraction time again.
Patent CN1706836A discloses a kind of method that separates fucoxanthine from marine alga, and the method is by the lixiviate in the dark of marine alga dimethyl sulfoxide (DMSO), then uses ethyl acetate and (NH
4)
2sO
4solution is extracted into the fucoxanthine in vat liquor in ethyl acetate, obtains the fucoxanthine of higher degree finally by 3～4 silica gel column chromatographies of mistake.This method has shortened extraction time compared with traditional method, the yield of fucoxanthine has also improved, but dimethyl sulfoxide (DMSO) is used as extraction solvent, in the time carrying out liquid-liquid extraction with ethyl acetate and ammonium sulfate, have in mutually residually in ethyl acetate, and dimethyl sulfoxide (DMSO) has high boiling point, and the method that can not distill by low-temperature reduced-pressure is removed, sample cannot be dried, and its existence can affect fucoxanthine purifying afterwards; And in this patent application, need repeatedly carry out silicagel column purifying to obtain the fucoxanthine product of high-content to the enriched material obtaining, a large amount of adsorption losses of target compound have been caused, increase again the complicacy of technique, if can once remove partial impurities in extraction process, contribute to simplify production technique.
But, because brown alga belongs to the special physiological structure of marine alga, there is the problems such as extraction efficiency is not high, consumption of organic solvent is large from wherein extracting fucoxanthine always, cause the waste of resource, again because organic solvent residual, affect greatly the quality of product.In view of above-mentioned these defects, can't meet the needs of actual production.Therefore, be necessary that invention is a kind of for from marine alga, particularly phaeophyta biology is prepared the technical skill of fucoxanthine, and the inventor, through lot of experiments, has completed the present invention finally.This technology comprises the pre-treatment, enzyme processing, extraction, separation of raw material, the content such as concentrated.
[summary of the invention]
[technical problem that will solve]
The object of this invention is to provide a kind of method that contains fucoxanthine enriched material of extracting from marine alga.
Another object of the present invention is to provide a kind of enriched material that contains fucoxanthine.
Another object of the present invention is to provide a kind of purposes of the enriched material that contains fucoxanthine.
[technical scheme]
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of method that contains fucoxanthine enriched material of extracting from marine alga.The step of the method is as follows:
A, raw materials pretreatment
Water washes away impurity and the salinity of marine alga remained on surface, under the condition of 30～50 DEG C of temperature and lucifuge, marine alga is dried, then is ground into seaweed powder;
B, enzyme processing
(1) get the water of 800～1400 weight parts, and water temperature is adjusted to 20～50 DEG C, then add 0.5～2.0 weight part cellulase and 0.1～0.4 weight part polygalacturonase, again with mineral acid or mineral alkali by the pH regulator to 4 of its solution～7, at 20～50 DEG C of temperature, activate 20～60min, so obtain a kind of enzyme treatment solution;
(2) enzyme treatment solution described in 30～500 weight parts is sprayed onto to 50～100 weight parts by steps A) in the seaweed powder that obtains, then stir, compacting, sealing, lucifuge insulation 4～96h at 20～50 DEG C of temperature, obtains a kind of enzyme and processes seaweed powder;
C, extraction
Taking 80～120 weight parts by step B) enzyme that obtains processes seaweed powder, under 2～50 DEG C of conditions of temperature, use 300～800 weight part 40～100% hydrophilic organic solvents to carry out refluxing extraction 30～90min, then separation and Extraction liquid, leftover materials repeat to extract 3～6 times, merge these extracting solutions;
D, from extracting solution, separate fucoxanthine
By step C) extracting solution that obtains mixes according to the volume ratio ratio of 6: 1～3: 1 with normal hexane, after concuss, standing separation 25～35min, separate lower floor's solution, residue upper solution repeats this step operation, until upper strata normal hexane is colourless mutually, merges these lower floor's solution;
Concentrating of E, fucoxanthine component
Under the condition of 40～55 DEG C of pressure-0.06～-0.095MPa and temperature, by step D) lower floor's solution of obtaining is concentrated into dryly, obtains the enriched material that contains fucoxanthine.
A preferred embodiment of the invention, described marine alga is selected from sea-tangle, Sargassum fusiforme, sargassun, bulk kelp, wakame or Thallus Gracilariae.
According to another kind of preferred implementation of the present invention, the granularity of described seaweed powder is 20～100 orders.
According to another kind of preferred implementation of the present invention, at step B) in use mineral acid be selected from hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid; Mineral alkali is selected from sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood, sodium bicarbonate or saleratus.
According to another kind of preferred implementation of the present invention, at step B) described in the enzyme work >=4000IU/g of cellulase, the enzyme work >=5000IU/g of described polygalacturonase.
According to another kind of preferred implementation of the present invention, at step C) described in hydrophilic organic solvent be selected from ethanol, methyl alcohol or acetone.
The invention still further relates to and adopt the enriched material that obtains of described method, it is characterized in that it contains more than 5% fucoxanthine in enriched material gross weight.
The invention still further relates to described enriched material in the purposes of preparing in foodstuff additive, functional foodstuff, medicine and fodder additives.
The present invention will be described below in more detail.
When the present invention extracts fucoxanthine from marine alga, first with cellulase and polygalacturonase, the marine alga of pulverizing is carried out to pre-treatment, destroy its cell wall structure, contribute to the release of activeconstituents, use again water-miscible organic solvent lixiviate 3～6 times, extracting solution is through liquid-liquid extraction, the impurity such as the chlorophyll existing in removal extracting solution, raffinate is through underpressure distillation, can obtain having the fucoxanthine condensed cream of certain content, this method extraction time is short, technique is simple, extraction efficiency is high, the product organic solvent-free obtaining is residual, comprehensive cost is cheap, for suitability for industrialized production provides production foundation.
The present invention relates to a kind of method that contains fucoxanthine enriched material of extracting from marine alga.The step of the method is as follows:
A, raw materials pretreatment
Water washes away impurity and the salinity of marine alga remained on surface, under the condition of 30～50 DEG C of temperature and lucifuge, marine alga is dried, then is ground into seaweed powder;
In the present invention, described marine alga is selected from the phaeophyta biologies such as sea-tangle, Sargassum fusiforme, sargassun, bulk kelp, wakame or Thallus Gracilariae;
Described marine alga all needs to desalt, the pre-treatment of impurity and pulverizing.
In the present invention, because fucoxanthine has the extremely unsettled feature of light and heat, therefore, clean marine alga need be dried lucifuge and the low temperature in the situation that.
In the present invention, when dry, can use normally used drying plant in Chinese medicinal materials processing technology to be dried, the GZX-9146MBE type digital display air dry oven that for example medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. produces is dried.
In the present invention, described pulverizing is to use normally used disintegrating apparatus in Chinese medicinal materials processing technology to carry out high speed shear pulverizing to marine alga, is crushed to 20～100 orders.
In the present invention, the pulverizer using can be the normally used pulverizer of selling in the market in Chinese medicinal materials processing technology, the food masher that for example Xin You of Jiangyin City Machinery Manufacturing Co., Ltd. produces.Typically use pulverizer raw material pulverizing is arrived to certain particle size, then sieve with standard medicine, collect 20～100 object seaweed powders.
B, enzyme processing
(1) get 800～1400 weight parts waters and water temperature is adjusted to 20～50 DEG C, then add 0.5～2.0 weight part cellulase and 0.1～0.4 weight part polygalacturonase, again with mineral acid or mineral alkali by the pH regulator to 4 of its solution～7, at 20～50 DEG C of temperature, activate 20～60min, so obtain a kind of enzyme treatment solution.
Cellulase (EC 3.2.1.4) is a kind of important enzyme product, is a kind of prozyme, is mainly made up of circumscribed beta-glucanase, Endo-β-glucanase and beta-glucosidase etc.Conventionally, cellulase is divided into three classes: C1 enzyme, Cx enzyme and beta-glucosidase enzyme.C1 enzyme is the enzyme at first Mierocrystalline cellulose being worked, and destroys the crystalline texture of cellulose chain.Cx enzyme is to act on through the Mierocrystalline cellulose of C1 enzyme activation, the cellulase of decomposition β-Isosorbide-5-Nitrae-glycosidic link.Beta-glucosidase enzyme can be decomposed into glucose by cellobiose, procellose and other low molecule cellodextrins.
In the present invention, described cellulase is for example Pangbo Bioengineering Co Ltd, Nanning's production of cellulose enzyme.
According to the present invention, if the enzyme work of described cellulase is lower than 4000IU/g, can be not high because of enzyme activity, and need to ensure that raw material cell wall broken wall is abundant with a large amount of cellulases, therefore the enzyme work of described cellulase should, higher than 4000IU/g, be lived in view of the enzyme of the cellulase of selling on market, and the enzyme work of described cellulase is 4000～10000IU/g, preferably 5000～9000IU/g, more preferably 6000～8000IU/g.
Wherein, enzyme work be defined as 1g enzyme powder or 1mL enzyme liquid in 40 DEG C with the condition of pH4.6 under, the enzyme amount that 1h decomposing soluble starch produces 1mg glucose is 1 Ge Meihuo unit.
Described polygalacturonase is a multienzyme complex of decompose pectin, generally includes protopectinase, pectinesterase lytic enzyme, pectinesterase.By their combined action, pectin substance is decomposed completely.Natural pectin substance, under protopectinase effect, changes into the pectin of water dissolvable; Pectin, by pectinesterase lytic enzyme catalytic elimination methyl esters group, generates pectic acid; Pectic acid generates galacturonic acid through polygalacturonase class and the degraded of pectate lyase class.
In the present invention, described polygalacturonase is for example the polygalacturonase that Pangbo Bioengineering Co Ltd, Nanning produces.
According to the present invention, if the enzyme work of described polygalacturonase is lower than 5000IU/g, can be not high because of enzyme activity, and need to ensure pectin contained raw material to be all hydrolyzed to ensure that target compound is better discharged with a large amount of polygalacturonases, therefore, the enzyme work of described polygalacturonase should be higher than 5000IU/g; In view of the enzyme work of the polygalacturonase of selling on the market, therefore the enzyme work of described polygalacturonase is 5000～12000IU/g, preferably 6000～10000IU/g, more preferably 8000～9000IU/g.
Preferably, dissolve 0.8～1.8 weight part cellulase and 0.15～0.35 weight part polygalacturonase with 800～1400 weight parts waters; Preferred, with 800～1400 weight parts waters dissolving 1.0～1.6 weight part cellulases and 0.2～0.3 weight part polygalacturonases.
In this step, the mineral acid of use is selected from hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid, is preferably selected from hydrochloric acid, sulfuric acid or phosphoric acid; More preferably be selected from hydrochloric acid or phosphoric acid.
In this step, the mineral alkali using is selected from sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood, sodium bicarbonate or saleratus, preferably be selected from sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate or saleratus, be more preferably selected from sodium hydroxide, sodium carbonate, sodium bicarbonate or saleratus.
In this step, cellulase and polygalacturonase are common enzyme in plant materials, it can ensure that the pH scope of enzyme activity is 4～7, in order to ensure the maximum vigor of enzyme in reaction process, the pH of reaction solution can not be too high, can not be too low, therefore, need to be with mineral acid or mineral alkali by the pH regulator to 4 of its enzyme solution～7.Too high or too low pH can make enzyme suffer irreversible breaking because affecting the stability of enzyme, thereby affects reaction effect.
(2) enzyme treatment solution described in 30～500 weight parts is sprayed onto to 50～100 weight parts by steps A) in the seaweed powder that obtains, then stir, compacting, sealing, lucifuge insulation 4～96h at 20～50 DEG C of temperature, obtains a kind of enzyme and processes seaweed powder.
In the present invention, use common mechanical stirrer or whipping device by described enzyme treatment solution with by steps A) in the seaweed powder that obtains mix, then use compact machine equipment will mix the density of mixture improve, then seal with plastic material, to can reach light-shading effect.In the present invention, the heat-preserving equipment using can be the thermostat water bath often using in experimentation, as the DZKW-C type electronic thermostatic water-bath of Beijing Hua Bolian medical apparatus corporation, Ltd production.
In this step, preferably use enzyme treatment solution and 50～100 weight parts described in 50～300 weight parts by steps A) seaweed powder that obtains.More preferably use enzyme treatment solution and 50～100 weight parts described in 75～200 weight parts by steps A) seaweed powder that obtains.
In this step, preferably, the mixture of described enzyme treatment solution and seaweed powder is lucifuge insulation 10～85h at 25～45 DEG C of temperature.More preferably, the mixture of described enzyme treatment solution and seaweed powder lucifuge insulation 20～75h at 30～40 DEG C of temperature.
C, extraction
Taking 80～120 weight parts by step B) enzyme that obtains processes seaweed powder, under 2～50 DEG C of conditions of temperature, use the hydrophilic organic solvent of 300～800 weight parts 40～100% to carry out refluxing extraction 30～90min, then separation and Extraction liquid, leftover materials repeat to extract 3～6 times, united extraction liquid.
Described hydrophilic organic solvent is selected from ethanol, methyl alcohol or acetone etc.They are all the solvents very generally using in chemical technology field, and are product solds in the market.
In the present invention, the extraction element using is the RE-5210A type Rotary Evaporators of being produced by Shanghai Zhen Jie experimental installation company limited, capacity is 10L, and vacuum pump is SHZ-D (III) the type circulating water type vacuum pump of being produced by Yuhua Instrument Co., Ltd., Gongyi City.
D, from extracting solution, separate fucoxanthine
By step C) extracting solution that obtains mixes according to the volume ratio ratio of 6: 1～3: 1 with normal hexane, after concuss, standing separation 25～35min, separate lower floor's solution, residue upper solution repeats this step operation, until upper strata normal hexane is colourless mutually, merges these lower floor's solution;
In the present invention, in the time carrying out liquid-liquid extraction with normal hexane and described extracting solution, in order to ensure in the situation that normal hexane consumption is minimum clean the Impurity removals such as chlorophyll, need follow a small amount of principle repeatedly, described extracting solution and normal hexane are advisable according to the volume ratio ratio of 6: 1～3: 1, be preferably 5: 1～4: 1, guarantee that removal of impurities is complete, reduce again solvent waste.
In the time that the present invention is used for industrial amplification production, can adopt high-speed counter-current extraction equipment to replace described concussion extraction.
Concentrating of E, fucoxanthine component
Under the condition of 40～55 DEG C of pressure-0.06～-0.09MPa and temperature, by step D) lower floor's solution of obtaining is concentrated into dryly, obtains containing fucoxanthine enriched material.
The enriched material obtaining adopts HPLC method to detect in a conventional manner the content of fucoxanthine.
The invention still further relates to and adopt the enriched material that obtains of described method, it is characterized in that it contains more than 5% fucoxanthine in enriched material gross weight.
Described enriched material, except fucoxanthine, also contains a certain amount of oil-soluble impurities.
The invention still further relates to described enriched material in the purposes of preparing in foodstuff additive, functional foodstuff, medicine and fodder additives.
Be noted that can be according to country the relevant regulations in foodstuff additive, functional foodstuff, medicine and feed additive field use and add the enriched material that the present invention contains fucoxanthine.
[beneficial effect]
The invention has the beneficial effects as follows:
1, extraction time is short, extracts fucoxanthine efficiency high;
Because fucoxanthine is the pigment being present in alginic cell, if directly marine alga is extracted with ethanol equal solvent, due to the intrinsic constructional feature of cell and osmotic pressure problem, be difficult to fucoxanthine to extract.In the present invention, marine alga is through the pre-treatment of enzyme liquid, and by obstinate cell walls disorganization, in marine alga, the composition such as contained carotenoid exists with free state form.And fucoxanthine has good solubility in ethanol, in the time refluxing lixiviate with ethanol, fucoxanthine can be discharged into rapidly and extract in solvent, has shortened greatly extraction time, and has improved extraction efficiency.
2, the product organic solvent-free obtaining is residual;
In the present invention, leaching process solvent used is ethanol, sepn process adopts normal hexane and the mode of extracting solvent liquid-liquid extraction to remove impurity, solvent for use kind is few, and both can reach good separation by the mode that regulates alcohol concn, therefore, in products obtained therefrom, organic solvent-free residual, product quality is guaranteed.
3, technique is simple, and comprehensive cost is cheap, is suitable for suitability for industrialized production
In the present invention, raw material is the phaeophyta marine algas such as sea-tangle, Sargassum fusiforme, sargassun, bulk kelp, wakame or Thallus Gracilariae, there is rich in natural resources in China, raw material easily obtains, and this technique is simple, after enzyme is processed, can largely wherein contained fucoxanthine be extracted with ethanol, separate with n-hexane extraction again, after concentrated, can obtain having the fucoxanthine enriched material of using value, avoid the use of a large amount of organic solvents in prior art, and be simplified from technique, also saved to a certain extent production cost.This technique strong operability aborning, has good industry and amplifies prospect.
[embodiment]
embodiment 1: the preparation that the present invention contains fucoxanthine enriched material
Implementation step is as follows:
A, raw materials pretreatment
Water is rinsed impurity residual sea-tangle top layer and salinity well, and be placed in medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. produce GZX-9146MBE type air dry oven, at 35 DEG C of temperature, dry, take the dry sea-tangle of 1kg, through be crushed to≤20 orders of high speed shear.
B, enzyme processing
(1) get 1000g water and water temperature is adjusted to 30 DEG C, then add the cellulase of 1.0g Pangbo Bioengineering Co Ltd, Nanning production and the polygalacturonase that 0.2g Pangbo Bioengineering Co Ltd, Nanning produces, again with hydrochloric acid or sodium hydroxide dilute aqueous soln by the pH regulator to 6.0 of its solution, at 30 DEG C of temperature, activate 40min, so obtain a kind of enzyme treatment solution;
(2) 1400 grams of described enzyme treatment solutions are sprayed onto to 700g by steps A) in the Kelp Powder that obtains, in 3000mL large beaker, add material on one side, spray enzyme treatment solution on one side, stir again, compacting, seal with preservative film, in the thermostat water bath of 30 DEG C of temperature, lucifuge insulation 60h, obtains a kind of enzyme and processes Kelp Powder;
C, extraction
Taking 100g at step B) enzyme that obtains processes Kelp Powder, join in 10L Rotary Evaporators, under 20 DEG C of conditions of temperature, using 400g concentration is that 80% ethanol carries out refluxing extraction 70min, then separation and Extraction liquid, leftover materials repeat to extract 5 times again, merge these extracting solutions;
D, from extracting solution, separate fucoxanthine
By step C) extracting solution that obtains mixes with 400g normal hexane, and after concuss, standing separation 30min, separates lower floor's solution, and residue upper solution repeats aforesaid operations, is colourless mutually to upper strata normal hexane, merges these lower floor's solution;
Concentrating of E, fucoxanthine component
Under the condition of 40 DEG C of pressure 0.095MPa and temperature, by step D) lower floor's solution of obtaining is concentrated into dryly, obtains the enriched material that contains fucoxanthine.Adopting HPLC method to detect in a usual manner its fucoxanthine content is 6.41%.
embodiment 2: the preparation of the enriched material that the present invention contains fucoxanthine
Implementation step is as follows:
A, raw materials pretreatment
Water is rinsed impurity residual sargassun top layer and salinity well, and be placed in medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. produce GZX-9146MBE type air dry oven, at 30 DEG C of temperature, dry, take the dry sargassun of 1kg, through be crushed to≤20 orders of high speed shear.
B, enzyme processing
(1) get 800g water and water temperature is adjusted to 40 DEG C, then add the cellulase of 0.5g Pangbo Bioengineering Co Ltd, Nanning production and the polygalacturonase that 0.4g Pangbo Bioengineering Co Ltd, Nanning produces, again with hydrochloric acid or sodium hydroxide dilute aqueous soln by the pH regulator to 5.0 of its solution, at 40 DEG C of temperature, activate 50min, so obtain a kind of enzyme treatment solution;
(2) 2700 grams of described enzyme treatment solutions are sprayed onto to 900g by steps A) in the sargassun powder that obtains, in bucket, add material on one side, spray enzyme treatment solution on one side, stir again, compacting, seal with preservative film, in the thermostat water bath of 40 DEG C of temperature, lucifuge insulation 30h, obtains a kind of enzyme and processes sargassun powder;
C, extraction
Taking 80g at step B) enzyme that obtains processes sargassun powder, join in 10L Rotary Evaporators, under temperature 50 C condition, using 300g concentration is that 40% ethanol carries out refluxing extraction 30min, then separation and Extraction liquid, leftover materials repeat to extract 6 times again, merge these extracting solutions;
D, from extracting solution, separate pheophytin
By step C) extracting solution that obtains mixes with 600g normal hexane, and after concuss, standing separation 30min, separates lower floor's solution, and residue upper solution repeats to upper strata normal hexane, mutually for colourless, to merge these lower floor's solution;
Concentrating of E, fucoxanthine component
Under the condition of pressure 0.095MPa and temperature 45 C, by step D) obtain lower floor's solution and be concentrated into dryly, obtain the enriched material that contains fucoxanthine.Adopting HPLC method to detect in a usual manner its fucoxanthine content is 6.93%.
embodiment 3: the preparation of the enriched material that the present invention contains fucoxanthine
Implementation step is as follows:
A, raw materials pretreatment
Water is rinsed impurity residual wakame top layer and salinity well, and be placed in medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. produce GZX-9146MBE type air dry oven, under temperature 50 C, dry, take 1kg dried undaria pinnatifida, through be crushed to≤20 orders of high speed shear.
B, enzyme processing
(1) get 1200g water and water temperature is adjusted to 50 DEG C, then add the cellulase of 1.5g Pangbo Bioengineering Co Ltd, Nanning production and the polygalacturonase that 0.3g Pangbo Bioengineering Co Ltd, Nanning produces, again with hydrochloric acid or sodium hydroxide dilute aqueous soln by the pH regulator to 7.0 of its solution, under temperature 50 C, activate 60min, so obtain a kind of enzyme treatment solution;
(2) 5000 grams of described enzyme treatment solutions are sprayed onto to 1000g by steps A) in the undaria powder that obtains, in bucket, add material on one side, spray enzyme treatment solution on one side, stir again, compacting, seal with preservative film, in the thermostat water bath of temperature 50 C, lucifuge insulation 4h, obtains a kind of enzyme and processes undaria powder;
C, extraction
Taking 120g at step B) enzyme that obtains processes undaria powder, join in 10L Rotary Evaporators, under 2 DEG C of conditions of temperature, using 800g concentration is that 100% ethanol carries out refluxing extraction 90min, then separation and Extraction liquid, leftover materials repeat to extract 3 times again, united extraction liquid;
D, from extracting solution, separate pheophytin
By step C) extracting solution that obtains mixes with 500g normal hexane, and after concuss, standing separation 30min, separates lower floor's solution, and it is colourless mutually that residue upper solution repeats aforesaid operations to upper strata normal hexane, merges these lower floor's solution;
Concentrating of E, fucoxanthine component
Under the condition of pressure 0.095MPa and temperature 50 C, by step D) lower floor's solution of obtaining is concentrated into dryly, obtains the enriched material that contains fucoxanthine.Adopting HPLC method to detect in a usual manner its fucoxanthine content is 5.79%.
embodiment 4: the preparation of the enriched material that the present invention contains fucoxanthine
Implementation step is as follows:
A, raw materials pretreatment
Water is rinsed impurity residual sea-tangle top layer and salinity well, and be placed in medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. produce GZX-9146MBE type air dry oven, at 40 DEG C of temperature, dry, take the dry sea-tangle of 1kg, through be crushed to≤20 orders of high speed shear.
B, enzyme processing
(1) get 1400g water and water temperature is adjusted to 20 DEG C, then add the cellulase of 2.0g Pangbo Bioengineering Co Ltd, Nanning production and the polygalacturonase that 0.1g Pangbo Bioengineering Co Ltd, Nanning produces, again with hydrochloric acid or sodium hydroxide dilute aqueous soln by the pH regulator to 4.0 of its solution, at 20 DEG C of temperature, activate 20min, so obtain a kind of enzyme treatment solution;
(2) 300 grams of described enzyme treatment solutions are sprayed onto to 500g by steps A) in the Kelp Powder that obtains, in 3000mL large beaker, add material on one side, spray enzyme treatment solution on one side, stir again, compacting, seal with preservative film, in the thermostat water bath of 20 DEG C of temperature, lucifuge insulation 96h, obtains a kind of enzyme and processes Kelp Powder;
C, extraction
Taking 110g at step B) enzyme that obtains processes Kelp Powder, join in 10L Rotary Evaporators, under 40 DEG C of conditions of temperature, using 600g concentration is that 60% ethanol carries out refluxing extraction 50min, then separation and Extraction liquid, leftover materials repeat to extract 4 times again, united extraction liquid;
D, from extracting solution, separate pheophytin
By step C) extracting solution that obtains mixes with 600g normal hexane, and after concuss, standing separation 30min, separates lower floor's solution, and it is colourless mutually that residue upper solution repeats aforesaid operations to upper strata normal hexane, merges these lower floor's solution;
Concentrating of E, fucoxanthine component
Under the condition of 55 DEG C of pressure 0.095MPa and temperature, by step D) lower floor's solution of obtaining is concentrated into dryly, obtains the enriched material that contains fucoxanthine.Adopting HPLC method to detect in a usual manner its fucoxanthine content is 5.86%.
Claims (8)
1. from marine alga, extract a method that contains fucoxanthine enriched material, it is characterized in that the step of the method is as follows:
A, raw materials pretreatment
Water washes away impurity and the salinity of marine alga remained on surface, under the condition of 30～50 DEG C of temperature and lucifuge, marine alga is dried, then is ground into seaweed powder;
B, enzyme processing
(1) get the water of 800～1400 weight parts, and water temperature is adjusted to 20～50 DEG C, then add 0.5～2.0 weight part cellulase and 0.1～0.4 weight part polygalacturonase, again with mineral acid or mineral alkali by the pH regulator to 4 of its solution～7, at 20～50 DEG C of temperature, activate 20～60min, so obtain a kind of enzyme treatment solution;
(2) enzyme treatment solution described in 30～500 weight parts is sprayed onto to 50～100 weight parts by steps A) in the seaweed powder that obtains, then stir, compacting, sealing, lucifuge insulation 4～96h at 20～50 DEG C of temperature, obtains a kind of enzyme and processes seaweed powder;
C, extraction
Taking 80～120 weight parts by step B) enzyme that obtains processes seaweed powder, under 2～50 DEG C of conditions of temperature, use the hydrophilic organic solvent that 300～800 weight part concentration are 100% to carry out refluxing extraction 30～90min, then separation and Extraction liquid, leftover materials repeat to extract 3～6 times, merge these extracting solutions;
D, from extracting solution, separate fucoxanthine
By step C) extracting solution that obtains mixes according to the ratio of volume ratio 6:1～3:1 with normal hexane, adopts high-speed counter-current extraction equipment to obtain lower floor's solution;
Concentrating of E, fucoxanthine component
Under the condition of 40～55 DEG C of pressure-0.06～-0.095MPa and temperature, by step D) lower floor's solution of obtaining is concentrated into dryly, obtains the enriched material that contains fucoxanthine.
2. method according to claim 1, is characterized in that described marine alga is selected from sea-tangle, Sargassum fusiforme, sargassun, bulk kelp, wakame or Thallus Gracilariae.
3. method according to claim 1, the granularity that it is characterized in that described seaweed powder is 20～100 orders.
4. method according to claim 1, is characterized in that at step B) in use mineral acid be selected from hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid; Mineral alkali is selected from sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood, sodium bicarbonate or saleratus.
5. method according to claim 1, is characterized in that at step B) described in the enzyme work >=4000IU/g of cellulase, the enzyme work >=5000IU/g of described polygalacturonase.
6. method according to claim 1, is characterized in that at step C) in, described hydrophilic organic solvent is selected from ethanol, methyl alcohol or acetone.
7. the enriched material obtaining according to method described in any one claim in claim 1～6, is characterized in that it contains more than 5% fucoxanthine in enriched material gross weight.
According to claim 7 enriched material in the purposes of preparing in foodstuff additive, functional foodstuff, medicine and fodder additives.
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| CN104254524B (en) * | 2012-04-27 | 2016-11-23 | 株式会社钟化 | The manufacture method of the compositions containing fucoxanthine |
| CN103012327B (en) * | 2012-12-21 | 2015-05-13 | 国家海洋局第三海洋研究所 | Preparation method of fucoxanthin |
| CN103232552B (en) * | 2013-04-24 | 2015-08-19 | 集美大学 | A kind of enzyme process prepares the method for brown alga fucosan and fucoxanthin |
| CN105287648B (en) * | 2015-11-05 | 2019-02-12 | 广东医学院 | Extraction and preparation method and application of active ingredients of sea hair cabbage |
| CN106566760A (en) * | 2016-11-08 | 2017-04-19 | 云南爱尔康生物技术有限公司 | Fucoxanthin healthcare wine and preparation method thereof |
| CN107188870A (en) * | 2017-06-29 | 2017-09-22 | 厦门理工学院 | A kind of method that fucoxanthin is extracted from brown alga |
| CN107382912B (en) * | 2017-07-31 | 2020-04-03 | 中国科学院海洋研究所 | A kind of method for improving fucoxanthin purity of sargassum crude extract |
| CN107581434A (en) * | 2017-10-27 | 2018-01-16 | 山东省农业科学院生物技术研究中心 | A kind of lactic acid bacteria beverage rich in astaxanthin and preparation method thereof |
| CN110560474B (en) * | 2019-09-05 | 2021-05-14 | 王旭 | Method for removing total chromium pollutants in chromium-polluted soil by water removal |
| CN115530372B (en) * | 2022-10-09 | 2024-01-30 | 北京姿美堂生物技术股份有限公司 | Seaweed extract with lipid-lowering function, preparation method thereof and seaweed extract composition |
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