CN110526949A - A kind of preparation method of the fine and soft anti-oxidant oligosaccharides in sea - Google Patents
A kind of preparation method of the fine and soft anti-oxidant oligosaccharides in sea Download PDFInfo
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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Abstract
The invention discloses a kind of preparation methods of the fine and soft anti-oxidant oligosaccharides in sea, including extract the fine and soft Thick many candies in sea, double alcohol precipitations are carried out to it and carry out cracking to extra large fine and soft polysaccharide using hydrogen peroxide obtaining the fine and soft oligosaccharides in sea.Young pilose antler activated oligosaccharide in the Antarctic Ocean prepared by the present invention is with high purity, antioxidant activity is strong, has ideal moisturizing rate and transdermal absorption factor, may be used on cosmetic field.Present invention process is simple, and the application for being Antarctic Ocean young pilose antler in cosmetics provides corresponding technological means.
Description
Technical field
The present invention relates to a kind of preparation methods of the fine and soft anti-oxidant oligosaccharides in sea.
Background technique
The Antarctic Ocean is fine and soft be mainly grown on the Antarctic Continent nearby, the pollution-free rock sea area of southern Chile, nutrition rich in
Substance, wherein polyoses content is higher.Research shows that plant polyose has bioactivity abundant in terms of cosmetics, there is antioxygen
Change, skin histology reparation, sun-proof, moisture retention, promotes the effects of skin blood circulation, anti-acne, immune enhancing at anti-aging, can
For playing the effect for improving skin environment, skin makeup skin care in cosmetics.Plant polyose has can not than other cosmetic materials
The advantages of analogy, its almost non-toxic side effect, function is efficient extensively, and good with most of cosmetic composition compatibility, so
It is very big that polysaccharide develops cosmetics potentiality.Existing many document reports application of the polysaccharide in terms of cosmetics, as spirulina is more
Sugar, hyaluronic acid, chitin and its derivative etc..
Currently on the market whitening spot-removing, anti-aging skin care item effective component mainly, chloro amido mercury and various phenols
Derivative often has certain harmfulness to skin.Developing has the fine and soft polysaccharide in the sea of anti-oxidation efficacy, and south not only can be improved
The extremely fine and soft added value in sea, and it is wider using providing in the cosmetic industries such as whitening spot-removing, anti-aging to be Antarctic Ocean young pilose antler
Wealthy space.
Summary of the invention
The present invention in view of the deficiencies of the prior art, using hydrogen peroxide cracks extra large fine and soft polysaccharide, specific summary of the invention
It is as follows:
A kind of preparation method of the fine and soft anti-oxidant oligosaccharides in sea, includes the following steps:
(1) the fine and soft Thick many candies in sea extract: using the Na of 1wt%-8wt%2CO3Solution extracts the fine and soft Thick many candies in sea, sea young pilose antler dry
Matter and Na2CO3The mass ratio of solution is 1:30-1:100, and reaction temperature is 30-80 DEG C, reaction time 2-8h, and reaction is completed
PH value is adjusted afterwards to neutrality, and extra large fine and soft Thick many candies are obtained by alcohol precipitation mode；
(2) purify: alcohol precipitation obtains extra large fine and soft polysaccharide again after the fine and soft Thick many candies redissolution in the sea that step (1) obtains；
(3) it cracks: cracking being carried out to extra large fine and soft polysaccharide using hydrogen peroxide and obtains the fine and soft oligosaccharides in sea, the additive amount of hydrogen peroxide
For 0.1wt%-5wt%, the additive amount of the fine and soft polysaccharide in the sea that step (2) obtains is 0.3 wt%-3wt%, and surplus is water；Reaction temperature
Degree is 50-80 DEG C, and the time in reaction time is 30-120min.
The alcohol that alcohol precipitation uses in step (1) and step (2) is preferably ethyl alcohol, and redissolving the solvent used is water.Step (2)
Described in the additive amount of the fine and soft polysaccharide in sea be the fine and soft polysaccharide dry matter additive amount in sea.
Preferably, the additive amount of hydrogen peroxide described in step (3) is 0.75wt%-1.25wt%, the fine and soft polysaccharide in sea
Additive amount be 0.5wt%-2wt%.
Preferably, Na described in step (1)2CO3Solution, concentration 2wt%-6wt%；The reaction temperature is 45
℃-70℃；The reaction time is 3-5h.
Preferably, the fine and soft oligosaccharides in sea that step (3) obtain is filtered using the filter membrane that aperture is 500D-10kD.
Preferably, the extraction raw material of the fine and soft Thick many candies in sea is the fine and soft dry powder in sea.The fine and soft dry powder in sea includes ovendry power and freeze-drying
Powder.
A kind of fine and soft oligosaccharides in sea, is prepared by above-mentioned preparation method, is had effects that oxidation resistant.
The invention has the following beneficial effects:
Young pilose antler activated oligosaccharide in the Antarctic Ocean prepared by the present invention is with high purity, antioxidant activity is strong, with ideal moisturizing rate and thoroughly
Skin absorptivity, may be used on cosmetic field.Present invention process is simple, and the application for being Antarctic Ocean young pilose antler in cosmetics provides phase
The technological means answered.
Detailed description of the invention
Fig. 1 is that the fine and soft oligosaccharides different pore size film in sea flows out component high performance liquid chromatography molecular weight determination in embodiment 1；
Fig. 2 is that different pore size film flows out the measurement of component Scavenging activity on hydroxyl free radical in embodiment 1；
Fig. 3 is that different pore size film flows out the measurement of component superoxide anion scavenging capacity in embodiment 1；
Fig. 4 is different component sucting wet curve (relative humidity 81%) in embodiment 1；
Fig. 5 is different component sucting wet curve (relative humidity 32%) in embodiment 1；
Fig. 6 is different component skin moisture content change curve in embodiment 1；
Fig. 7 is Transdermal absorption experimental provision schematic diagram in embodiment 1；
Fig. 8 is different component residual moisture curve (relative humidity 0%) in embodiment 1；
In Fig. 1: A, hydrogen peroxide pyrolysis product, B, H1- molecular cut off 500Da film effluent, C, H2- retain molecule
Measure 1kDa film effluent, D, H3- molecular cut off 3kDa film effluent, E, H4 molecular cut off 5kDa film effluent, F, H5-
Molecular cut off 10kDa film effluent；
In Fig. 7: 1, supply pool；2, sample tap；3, acceptance pool；4, stirrer.
Specific embodiment
Principles and features of the present invention are described below in conjunction with example, the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.
Embodiment 1
A kind of preparation method of the fine and soft anti-oxidant oligosaccharides in sea, includes the following steps:
(1) the fine and soft Thick many candies in sea extract: using extra large fine and soft dry powder as raw material, using the Na of 4wt%2CO3It is fine and soft thick more that solution extracts sea
Sugar, sea young pilose antler dry matter and Na2CO3The mass ratio of solution is 1:50, and reaction temperature is 60 DEG C, reaction time 4h, and reaction is completed
PH value is adjusted afterwards to neutrality；8000r/m centrifugation 6min takes supernatant, and supernatant is concentrated to the 1/10 of original volume；By concentration
The 95wt% ethyl alcohol of its 4 times of volumes is added in supernatant, and 4 DEG C stand 12 hours, and 8000r/m is centrifuged 6min, collect precipitating, dries
It is dry, obtain extra large fine and soft Thick many candies；
(2) purify: alcohol precipitation obtains extra large fine and soft polysaccharide again after the Antarctic Ocean young pilose antler Thick many candies redissolution that step (1) obtains；Specific behaviour
As: the water that 3 times of its quality is added in the fine and soft Thick many candies in sea that step (1) obtains is redissolved, extra large fine and soft Thick many candies solution is obtained；Xiang Hairong
The 95wt% ethyl alcohol of its 4 times of volumes is added in Thick many candies solution, and 4 DEG C stand 12 hours, and 8000r/m is centrifuged 6min, collects precipitating；
Precipitating is washed with dehydrated alcohol, drying, is obtained extra large fine and soft polysaccharide, is saved backup in 4 DEG C.
(3) it cracks: cracking being carried out to extra large fine and soft polysaccharide using hydrogen peroxide and obtains the fine and soft oligosaccharides in sea.With antioxidation in vitro index
(superoxide anion inhibiting rate and hydroxy radical inhibiting rate) is standard, and (i.e. sea is fine and soft more for hydrogen peroxide additive amount, substrate additive amount
Sugared additive amount), reaction temperature, reaction time be single factor design orthogonal test, the single factor test optimal conditions of selection are as follows:
1 hydrogen peroxide method of table prepares oligosaccharides single factor test condition optimizing
It on the basis of single factor test condition, is freeze-dried for 24 hours, pulverizes spare, according to antioxidation in vitro after reaction
Activity carries out screening and carries out response surface experiment.
Superoxide anion, the detection of hydroxy radical inhibitory activity are carried out to each group embodiment component, detection method is as follows:
1. the measurement of ultra-oxygen anion free radical clearance rate
The ability for removing ultra-oxygen anion free radical uses assay NBT photoreduction, and pyrogallol is under alkaline condition
Autoxidation can occur, generate coloured intermediate product and ultra-oxygen anion free radical, ultra-oxygen anion free radical urges autoxidation
Change effect.The ultra-oxygen anion free radical kit that selection Nanjing is built up is detected, and replaces sample to do blank with distilled water
Inhibiting rate is calculated as follows in group.
Inhibiting rate=(A blank-A sample)/A blank × 100%
In formula: A sample, A blank are respectively the light absorption value of sample and blank.
2. the detection of Scavenging action to hydroxyl free radical
The measurement of Hydroxyl radical-scavenging ability is that the hydroxy radical detection kit built up by Nanjing is detected, In
Trap is measured at 520nm.Blank group replaces test sample with distilled water, and inhibiting rate is calculated as follows:
Inhibiting rate=(A sample-A blank)/(A control-A blank) × 100%
In formula: A sample, A blank, A control are respectively sample, blank and the light absorption value of control.
Comprehensive antioxidation activity in vitro screening single factor test condition optimizing is as follows, selects reaction time 60min, reaction temperature
50-80 DEG C, hydrogen peroxide additive amount 0.75-1.25%, substrate additive amount 0.5-2% carry out subsequent response surface analysis.
(4) response phase method screens optimal conditions: on the basis of single factor test, using in Design- Expert8.0.5
Box-Behnken center combination carry out Three factors-levels design response surface experiments, with temperature (A), substrate additive amount (B) and
Amount of hydrogen peroxide (C) is variable, and wherein temperature selects 50,65,80 DEG C, and substrate additive amount selects 0.5,1.25,2wt%, peroxide
Change hydrogen additive amount selection 0.75,1,1.25wt%, the reaction time is fixed as 60min, central point be repeated 5 times totally 17 handle
To following design scheme and result.17 treatment conditions and result situation are as shown in table 2.
The fine and soft oligosaccharides response surface in 2 hydrogen peroxide method of table preparation sea designs table
(5) preferred for superoxide anion and Scavenging activity on hydroxyl free radical maximum value progress condition, obtain best practice
Are as follows: according to substrate 1.32wt%, hydrogen peroxide additive amount 0.94wt%, 70 DEG C of reaction temperature, obtains the highest oligosaccharides of activity and mention
Object is taken, superoxide anion inhibiting rate is 39.38%, and Hydroxyl radical-scavenging inhibiting rate is 77.93%.
(6) filter membrane screens: cracking according to the above-mentioned optimal conditions filtered out to extra large fine and soft polysaccharide, obtains extra large fine and soft oligosaccharides
Solution filters extra large fine and soft mistake using the filter membrane (aperture is respectively 500Da, 1kDa, 3kDa, 5kDa, 10kDa) of different pore size respectively
Hydrogen oxide pyrolysis product obtains film effluent component H1, H2, H3, H4, H5 (molecular weight arranges from low to high), it is intended to will crack
Product carries out different molecular weight division, obtains the higher product oligosaccharides of active higher purity.The fine and soft peroxidating in different filter membrane outflows sea
Hydrogen pyrolysis product molecular weight determination carries out molecular weight determination using high performance liquid chromatography, and measurement result is shown in Fig. 1.
The smooth no miscellaneous peak of chromatograms as shown in Figure 1 illustrates that hydrogen peroxide cracking oligosaccharides purity is higher, passes through each aperture
The effluent of film should theoretically obtain the five groups of components of weight average molecular weight from low to high.But it can be with from high performance liquid chromatography result
It is very high to obtain hydrogen peroxide pyrolysis product cracking severity under this condition, product is that (molecular weight is less than the lesser oligosaccharides of molecular weight
The component accounting of 500Da is up to 98%).It is only capable of obtaining weight average molecular weight being 180Da's and 264Da by the film of different molecular weight
Pyrolysis product, H1 weight average molecular weight are 180Da, and it is 264Da, Bu Nengqu that H2, H3, H4, H5 product weight average molecular weight are close
Point, H1 is named as H-1, H2, H3, H4, H5 merging are named as H-2, in case subsequent experimental.
(7) superoxide anion different retention component antioxidation activity in vitro measurements: is measured to H1, H2, H3, H4, H5 respectively
Inhibiting rate and hydroxy radical inhibiting rate, measuring method are same as above, and as a result see Fig. 2, Fig. 3.The fine and soft hydrogen peroxide in sea as shown in Figure 2 and Figure 3
Lysate crosses film outflow component H2, H3, H4, H5 non-table in terms of Scavenging activity on hydroxyl free radical and superoxide anion scavenging capacity
Reveal notable difference, the result is consistent with high performance liquid chromatography molecular weight determination, cannot distinguish between by the film of different pore size
Several groups of components.H2, H3, H4, H5 antioxidant activity are apparently higher than H1.
(8) moisture absorbability and moisture retentivity measures: H-1, H-2 are placed in 105 DEG C of baking oven, it is sufficiently dry.Under 25 DEG C of constant temperature,
81% relative humidity (RH) is maintained with the saturated ammonium sulfate aqueous solution in drier, the saturation calcium chloride in drier is water-soluble
Liquid maintains 32% relative humidity (RH).0.5g each group sample is accurately weighed, the drier of different relative humidity is respectively placed in
In, using glycerol as control.Each sample weight is accurately weighed after at regular intervals, until taking out after 72h, measures hydroscopicity.
Hydroscopicity (%)=(Hn/H0) × 100%
Moisture content before Hn-- is placed
Moisture content after H0-- is placed
Moisture absorption situation of different component under the conditions of RH81% and RH32% is as shown in Figure 4, Figure 5, and wherein Z-1, Z-2 are
Similar control product.As shown, Antarctic Ocean young pilose antler different component all shows preferable hygroscopicity, In under the conditions of RH81%
Absorbability is lower under the conditions of RH32%, and is below glycerol hygroscopicity under corresponding conditions.Each component moisture absorption rate in preceding 30h
Higher, general cosmetics are that application of each component in cosmetic product is provided fundamental basis within for 24 hours using the time.
(9) body surface moisture retention measures:
Determination condition: 20 DEG C~25 DEG C of temperature, relative humidity 35%~70%；
Measuring method: each sample aqueous solution that configuration concentration is 1%, using 10% glycerol as object of reference.It selects at random
The skin health subject of 22~30 age brackets 10, choosing is recipient site at same area 5cm × 5cm on the inside of left forearm,
After cleaning, uniformly smear sample and reference solution, dosage 0.1mL, with moisture of skin tester measurement 0min, 10min,
After 30min, 60min, 120 min and smear before skin moisture content, in the same area choose difference measurement 3~4
It is secondary, the moisture content of measurement is subtracted into the measured value that the skin moisture content before not smearing is the period.Recipient site is real
Any skin care item cannot be used by testing first 2~3 days, and subject is required to enter test environment in advance, carry out experiment after rest again.
Experimental result is shown in Fig. 6.
As shown in figure 5, wherein Z-1, Z-2 are similar control product.It compares and smears glycerol and H-1, H-2 component skin
The moisture content change of different time, wherein converting using initial time skin moisture content as basic point.Preceding 10min due to
The sample and glycerol of smearing, which contain certain moisture, increases rapidly skin moisture content, with the extension moisture of skin of time
Content gradually decreases, and 120min inner skin moisture content is above initial content.H-2 body surface moisturizing activity is living compared with other oligosaccharides
Property is higher.
(10) percutaneous absorbability measures: take female KM mouse skin to give the Antarctic Ocean fine and soft different retention components in experiment,
The influence of time, molecular weight to transdermal absorption factor is investigated respectively by Transdermal absorption instrument.
Mouse skin is fixed between supply pool and acceptance pool, skin surface is upward.Using improved Franz diffusing cells method,
Using the physiological saline containing 0.5% sodium azide as acceptable solution, transdermal experiment is carried out under conditions of 32 DEG C, 600 r/min revolving speeds.
Transdermal area is 1.77cm2, acceptable solution volume is 6 mL, and transdermal device is as shown in Figure 7.
Choosing each molecular species is experimental subjects, and each group sample is configured to the solution of required concentration with acceptable solution, is taken
Supply pool is added in 1mL, in 2h, 4h, 6h, 8h, 10h, takes acceptable solution 1mL afterwards for 24 hours and is supplied with fresh acceptable solution.Measurement receives
The content of oligosaccharides in liquid, and unit of account area adds up transit dose, and then analysis time, molecular weight and concentration as follows
Influence to percutaneous absorbability.
The unit area of Qn:t time sample adds up transit dose (μ g/cm2)；A: infiltrating area (1.77cm2)；When Cn:t
Between concentration measurement；Concentration measurement before the Ci:t time；V: acceptable solution total volume (12mL)；V0: sample volume (1mL)；J:
Percutaneous rate constant.Make Qn and regression equation is obtained as curve to t, this equation slope is percutaneous rate constant.Experimental result is shown in Table
8。
The effect generated after function cosmetic applications be subjected to the physicochemical property of effective component and matrix, dosage form, concentration,
Application method, site of action, contact area, uses the factors such as duration, transdermal agent property and body condition at dosage
It influences (cosmetic industry evaluation).Transdermal absorption problem is always the premise of cosmetics efficiency evaluation, currently for small molecule
Transdermal absorption built consensus, so that more effective components is penetrated into cortexes, reach effective local concentration, so as to
The effect of improving cosmetics.Therefore our department's separating tests will investigate Antarctic Ocean young pilose antler activated oligosaccharide percutaneous absorbability, probe into its
The application for kind of making up.
As shown in figure 8, wherein Z-1, Z-2 are similar control product, Antarctic Ocean young pilose antler algae oligosaccharides different component has been investigated in matter
Measure the unit area Percutaneous permeability of Transdermal absorption for 24 hours when concentration is 10g/L.When for 24 hours difference oligosaccharide compositions show compared with
Good percutaneous absorbability, wherein the permeability of H-1 is slightly above H-2, this may be the barrier action due to cuticula, and molecular weight is got over
Small substance is easier to penetrate keratoderma.
By testing the further screening Antarctic Ocean young pilose antler component H-1 and H-2 above, molecular weight is respectively less than 500Da, because
This Antarctic Ocean young pilose antler oligosaccharides antioxidation activity in vitro with higher for dividing screening conditions to prepare with the present invention, preferable moisture absorption are protected
Wet activity, percutaneous absorbability are high.Compared with previous preparation method, product bioactivity is high, and preparation method is simple for of the invention preparing
It is single convenient, preferable application prospect is provided in cosmetic field for Antarctic Ocean young pilose antler oligosaccharides.
Embodiment 2
A kind of preparation method of the fine and soft anti-oxidant oligosaccharides in sea, includes the following steps:
(1) the fine and soft Thick many candies in sea extract: using extra large fine and soft dry powder as raw material, using the Na of 1wt%2CO3It is fine and soft thick more that solution extracts sea
Sugar, sea young pilose antler dry matter and Na2CO3The mass ratio of solution is 1:30, and reaction temperature is 80 DEG C, reaction time 8h, and reaction is completed
PH value is adjusted afterwards to neutrality；8000r/m centrifugation 6min takes supernatant, and supernatant is concentrated to the 1/10 of original volume；By concentration
The 95wt% ethyl alcohol of its 4 times of volumes is added in supernatant, and 4 DEG C stand 12 hours, and 8000r/m is centrifuged 6min, collect precipitating, dries
It is dry, obtain extra large fine and soft Thick many candies；
(2) purify: alcohol precipitation obtains extra large fine and soft polysaccharide again after the Antarctic Ocean young pilose antler Thick many candies redissolution that step (1) obtains；Specific behaviour
As: the water that 3 times of its quality is added in the fine and soft Thick many candies in sea that step (1) obtains is redissolved, extra large fine and soft Thick many candies solution is obtained；Xiang Hairong
The 95wt% ethyl alcohol of its 4 times of volumes is added in Thick many candies solution, and 4 DEG C stand 12 hours, and 8000r/m is centrifuged 6min, collects precipitating；
Precipitating is washed with dehydrated alcohol, drying, is obtained extra large fine and soft polysaccharide, is saved backup in 4 DEG C.
(3) it cracks: cracking being carried out to extra large fine and soft polysaccharide using hydrogen peroxide and obtains the fine and soft oligosaccharides in sea, the additive amount of hydrogen peroxide
For 0.1wt%, the additive amount of the fine and soft polysaccharide in the sea that step (2) obtains is 0.3wt%, and surplus is water；Reaction temperature is 50 DEG C, instead
The time is 120min between seasonable.
Embodiment 3
A kind of preparation method of the fine and soft anti-oxidant oligosaccharides in sea, includes the following steps:
(1) the fine and soft Thick many candies in sea extract: using extra large fine and soft dry powder as raw material, using the Na of 8wt%2CO3It is fine and soft thick more that solution extracts sea
Sugar, sea young pilose antler dry matter and Na2CO3The mass ratio of solution is 1:100, and reaction temperature is 30 DEG C, reaction time 2h, and reaction is completed
PH value is adjusted afterwards to neutrality；8000r/m is centrifuged 6 min and takes supernatant, and supernatant is concentrated to the 1/10 of original volume；By concentration
The 95wt% ethyl alcohol of its 4 times of volumes is added in supernatant, and 4 DEG C stand 12 hours, and 8000r/m is centrifuged 6min, collect precipitating, dries
It is dry, obtain extra large fine and soft Thick many candies；
(2) purify: alcohol precipitation obtains extra large fine and soft polysaccharide again after the Antarctic Ocean young pilose antler Thick many candies redissolution that step (1) obtains；Specific behaviour
As: the water that 3 times of its quality is added in the fine and soft Thick many candies in sea that step (1) obtains is redissolved, extra large fine and soft Thick many candies solution is obtained；Xiang Hairong
The 95wt% ethyl alcohol of its 4 times of volumes is added in Thick many candies solution, and 4 DEG C stand 12 hours, and 8000r/m is centrifuged 6min, collects precipitating；
Precipitating is washed with dehydrated alcohol, drying, is obtained extra large fine and soft polysaccharide, is saved backup in 4 DEG C.
(3) it cracks: cracking being carried out to extra large fine and soft polysaccharide using hydrogen peroxide and obtains the fine and soft oligosaccharides in sea, the additive amount of hydrogen peroxide
For 5wt%, the additive amount of the fine and soft polysaccharide in the sea that step (2) obtains is 3wt%, and surplus is water；Reaction temperature is 80 DEG C, when reaction
Between the time be 30min.
Embodiment 4
A kind of preparation method of the fine and soft anti-oxidant oligosaccharides in sea, includes the following steps:
(1) the fine and soft Thick many candies in sea extract: using extra large fine and soft dry powder as raw material, using the Na of 2wt%2CO3It is fine and soft thick more that solution extracts sea
Sugar, sea young pilose antler dry matter and Na2CO3The mass ratio of solution is 1:50, and reaction temperature is 45 DEG C, reaction time 5h, and reaction is completed
PH value is adjusted afterwards to neutrality；8000r/m centrifugation 6min takes supernatant, and supernatant is concentrated to the 1/10 of original volume；By concentration
The 95wt% ethyl alcohol of its 4 times of volumes is added in supernatant, and 4 DEG C stand 12 hours, and 8000r/m is centrifuged 6min, collect precipitating, dries
It is dry, obtain extra large fine and soft Thick many candies；
(2) purify: alcohol precipitation obtains extra large fine and soft polysaccharide again after the Antarctic Ocean young pilose antler Thick many candies redissolution that step (1) obtains；Specific behaviour
As: the water that 3 times of its quality is added in the fine and soft Thick many candies in sea that step (1) obtains is redissolved, extra large fine and soft Thick many candies solution is obtained；Xiang Hairong
The 95wt% ethyl alcohol of its 4 times of volumes is added in Thick many candies solution, and 4 DEG C stand 12 hours, and 8000r/m is centrifuged 6min, collects precipitating；
Precipitating is washed with dehydrated alcohol, drying, is obtained extra large fine and soft polysaccharide, is saved backup in 4 DEG C.
(3) it cracks: cracking being carried out to extra large fine and soft polysaccharide using hydrogen peroxide and obtains the fine and soft oligosaccharides in sea, the additive amount of hydrogen peroxide
For 0.75wt%, the additive amount of the fine and soft polysaccharide in the sea that step (2) obtains is 0.5wt%, and surplus is water；Reaction temperature is 80 DEG C, instead
The time is 30min between seasonable.
Embodiment 5
A kind of preparation method of the fine and soft anti-oxidant oligosaccharides in sea, includes the following steps:
(1) the fine and soft Thick many candies in sea extract: using extra large fine and soft dry powder as raw material, using the Na of 6wt%2CO3It is fine and soft thick more that solution extracts sea
Sugar, sea young pilose antler dry matter and Na2CO3The mass ratio of solution is 1:50, and reaction temperature is 70 DEG C, reaction time 3h, and reaction is completed
PH value is adjusted afterwards to neutrality；8000r/m centrifugation 6min takes supernatant, and supernatant is concentrated to the 1/10 of original volume；By concentration
The 95wt% ethyl alcohol of its 4 times of volumes is added in supernatant, and 4 DEG C stand 12 hours, and 8000r/m is centrifuged 6min, collect precipitating, dries
It is dry, obtain extra large fine and soft Thick many candies；
(2) purify: alcohol precipitation obtains extra large fine and soft polysaccharide again after the Antarctic Ocean young pilose antler Thick many candies redissolution that step (1) obtains；Specific behaviour
As: the water that 3 times of its quality is added in the fine and soft Thick many candies in sea that step (1) obtains is redissolved, extra large fine and soft Thick many candies solution is obtained；Xiang Hairong
The 95wt% ethyl alcohol of its 4 times of volumes is added in Thick many candies solution, and 4 DEG C stand 12 hours, and 8000r/m is centrifuged 6min, collects precipitating；
Precipitating is washed with dehydrated alcohol, drying, is obtained extra large fine and soft polysaccharide, is saved backup in 4 DEG C；
(3) it cracks: cracking being carried out to extra large fine and soft polysaccharide using hydrogen peroxide and obtains the fine and soft oligosaccharides in sea, the additive amount of hydrogen peroxide
For 1.25wt%, the additive amount of the fine and soft polysaccharide in the sea that step (2) obtains is 2wt%, and surplus is water；Reaction temperature is 65 DEG C, reaction
Time time is 60min.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of the fine and soft anti-oxidant oligosaccharides in sea, which comprises the steps of:
(1) the fine and soft Thick many candies in sea extract: using the Na of 1wt%-8wt%2CO3Solution extracts the fine and soft Thick many candies in sea, sea young pilose antler dry matter with
Na2CO3The mass ratio of solution is 1:30-1:100, and reaction temperature is 30-80 DEG C, and reaction time 2-8h is adjusted after the reaction was completed
PH value obtains extra large fine and soft Thick many candies by alcohol precipitation mode to neutrality；
(2) purify: alcohol precipitation obtains extra large fine and soft polysaccharide again after the fine and soft Thick many candies in sea that step (1) obtains are redissolved；
(3) it cracks: cracking being carried out to extra large fine and soft polysaccharide using hydrogen peroxide and obtains the fine and soft oligosaccharides in sea, the additive amount of hydrogen peroxide is
The additive amount of 0.1wt%-5wt%, the fine and soft polysaccharide in the sea that step (2) obtains are 0.3wt%-3wt%, and surplus is water；Reaction temperature
It is 50-80 DEG C, the time in reaction time is 30-120min.
2. preparation method according to claim 1, which is characterized in that the additive amount of hydrogen peroxide described in step (3) is
The additive amount of 0.75wt%-1.25wt%, the fine and soft polysaccharide in sea are 0.5wt%-2wt%.
3. preparation method according to claim 1, which is characterized in that Na described in step (1)2CO3Solution, concentration are
2wt%-6wt%；The reaction temperature is 45 DEG C -70 DEG C；The reaction time is 3-5h.
4. preparation method according to claim 1, which is characterized in that use aperture to the fine and soft oligosaccharides in sea that step (3) obtain
It is filtered for the filter membrane of 500D-10kD.
5. preparation method according to claim 1, which is characterized in that the extraction raw material of sea young pilose antler Thick many candies is the fine and soft dry powder in sea.
6. a kind of fine and soft oligosaccharides in sea, is prepared, which is characterized in that have by the described in any item preparation methods of claim 1-5
Oxidation resistant effect.
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Application publication date: 20191203 |