CN109879979A - A kind of antioxidant and preparation method thereof - Google Patents
A kind of antioxidant and preparation method thereof Download PDFInfo
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- CN109879979A CN109879979A CN201910170278.6A CN201910170278A CN109879979A CN 109879979 A CN109879979 A CN 109879979A CN 201910170278 A CN201910170278 A CN 201910170278A CN 109879979 A CN109879979 A CN 109879979A
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Abstract
The present invention discloses a kind of antioxidant and preparation method thereof, is related to antioxidant technology field.The antioxidant includes esterification rice bran polysaccharide.For the preparation method of the antioxidant the following steps are included: chlorosulfonic acid is added dropwise into anhydrous pyridine, reaction forms esterifying reagent；Rice bran polysaccharide, stirring to formation suspension system are added into n,N-Dimethylformamide；The esterifying reagent is added in the suspension system, stirring forms reaction solution；It adjusts after the reaction solution is in neutrality, is separated by solid-liquid separation, must be precipitated after 95% ethyl alcohol is added in Xiang Suoshu reaction solution；It dialyses after taking the precipitating to be dissolved in water, collects and retain liquid vacuum concentration, rice bran polysaccharide must be esterified after dry.Antioxidant produced by the present invention is more more stable than the property of rice bran polysaccharide, and has stronger anti-oxidation function, and be easy to be absorbed by organisms and have no toxic side effect to body.
Description
Technical field
The present invention relates to antioxidant technology field, in particular to a kind of antioxidant and preparation method thereof.
Background technique
In the case of the metabolism of organism has a kind of contradictory, although most of tellurian biology needs oxygen
It survives, but oxygen is a kind of molecule of high reaction activity again simultaneously, can produce reactive oxygen species, when activity in vivo oxygen produces
Raw excessive, antioxidant ability of organism decline or generation and purge mechanism are unbalance, it will be made to accumulate in vivo and cause cell
Oxidative damage.The active oxygen species generated in the cell include hydrogen peroxide, hypochlorous acid, free radical such as hydroxyl radical free radical and surpass
Oxide anion.Wherein, hydroxyl radical free radical is especially unstable, and energy nothing is specifically reacted with most of biomolecule rapidly,
Or O-DNA and protein breakdown cell.
Anti-oxidant is exactly any substance that there is the oxidation reaction that can effectively inhibit free radical with low concentration, acts on machine
Reason, which can be, acts directly on free radical, or consumes the substance for being easy to generate free radical indirectly, prevents further anti-
It answers.Current anti-oxidant substance includes natural (such as vitamin C, vitamin E) and artificial synthesized anti-oxidant
Agent.Wherein, artificial synthesized antioxidant is easy to produce toxicity due to metabolic stress, causes to damage to body, market is to natural
The demand of antioxidant is significantly increased.And natural extraction cost is higher and inevitably there is impurity, causes
Purity is lower, and due to mostly playing a role using monomeric form as effective component, is not only easy to be metabolized, but also anti-oxidant work
Property is lower.
Summary of the invention
The main object of the present invention is to propose a kind of antioxidant and preparation method thereof, it is intended to prepare it is a kind of it is safe and non-toxic,
Property is stable and has the antioxidant of good antioxidant activity.
To achieve the above object, the present invention proposes that a kind of antioxidant, the antioxidant include esterification rice bran polysaccharide.
To achieve the above object, the invention also provides a kind of preparation method of antioxidant, the systems of the antioxidant
Preparation Method the following steps are included:
Chlorosulfonic acid is added dropwise into anhydrous pyridine, reaction forms esterifying reagent；
Rice bran polysaccharide, stirring to formation suspension system are added into n,N-Dimethylformamide；
The esterifying reagent is added in the suspension system, stirring forms reaction solution；
It adjusts after the reaction solution is in neutrality, is separated by solid-liquid separation after 95% ethyl alcohol is added in Xiang Suoshu reaction solution,
It must precipitate；
It dialyses after taking the precipitating to be dissolved in water, collects and retain liquid vacuum concentration, rice bran polysaccharide must be esterified after dry.
Preferably, described that chlorosulfonic acid is added dropwise into anhydrous pyridine, react the step of forming esterifying reagent, comprising:
Reaction vessel equipped with anhydrous pyridine is placed in ice salt bath cooling；
Under ice salt bath, chlorosulfonic acid is slowly added dropwise into the reaction vessel while stirring, reaction forms esterifying reagent；
Wherein, the volume ratio of the chlorosulfonic acid and anhydrous pyridine is 1:(3~5).
Preferably, described under ice salt bath, chlorosulfonic acid is slowly added dropwise into the reaction vessel while stirring, reaction is formed
In the step of esterifying reagent, the temperature when reaction is 0~4 DEG C, and the time of the reaction is 0.5~2h.
Preferably, described that the esterifying reagent is added in the suspension system, formed reaction solution the step of in, it is described
The solid-to-liquid ratio (g:L) of rice bran polysaccharide and the esterifying reagent in suspension system is (5~7): 1.
Preferably, described that the esterifying reagent is added in the suspension system, it stirs in the step of forming reaction solution,
When the formation reaction solution, reaction temperature is 60~80 DEG C, and the reaction time is 1.5~2h.
Preferably, after the adjusting reaction solution is in neutrality, it is laggard that 95% ethyl alcohol is added in Xiang Suoshu reaction solution
The step of row is separated by solid-liquid separation, and obtains precipitating, comprising:
The pH that sodium hydroxide solution is added dropwise to the reaction solution into the reaction solution is 6.8~7.2, is obtained neutral molten
Liquid；
Then 95% ethyl alcohol is added into the neutral solution and forms mixed solution, when ethyl alcohol is in the mixed solution
When mass fraction is 70%, stop that 95% ethyl alcohol is added；
The mixed solution is centrifuged, must be precipitated.
Preferably, it is described into the reaction solution be added dropwise sodium hydroxide solution to the reaction solution pH be 6.8~
7.2, in the step of obtaining neutral solution, the concentration of the sodium hydroxide solution is 1~5mol/L.
Preferably, it is described take the precipitating to be dissolved in water after dialyse, collect and retain liquid vacuum concentration, must be esterified after dry
In the step of rice bran polysaccharide, the dialyzate used of dialysing is water.
Preferably, it is described take the precipitating to be dissolved in water after dialyse, collect and retain liquid vacuum concentration, must be esterified after dry
In the step of rice bran polysaccharide,
The dialysis time is 24~48h.
In technical solution of the present invention, use native compound rice bran polysaccharide for raw material, by being esterified to rice bran polysaccharide
Modification, obtained esterification rice bran polysaccharide is more more stable than the property of rice bran polysaccharide, and has stronger anti-oxidation function, and be easy to
It is absorbed by organisms and has no toxic side effect to body.To be esterified rice bran polysaccharide as antioxidant, raw material sources are huge and price is low
It is honest and clean, antioxidant cost is reduced well, develop and be utilized this precious resources of rice bran, be the application extension side of rice bran
To.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
Other relevant attached drawings are obtained according to these attached drawings.
Fig. 1 is the flow diagram of an embodiment of the preparation method of antioxidant provided by the invention；
Fig. 2 is the clearance rate variation comparison to OH free radical of antioxidant made from Examples 1 to 6 and rice bran polysaccharide
Figure.
The embodiments will be further described with reference to the accompanying drawings for the realization, the function and the advantages of the object of the present invention.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Current anti-oxidant substance includes natural (such as vitamin C, vitamin E) and artificial synthesized anti-
Oxidant.Wherein, artificial synthesized antioxidant is easy to produce toxicity due to metabolic stress, causes to damage to body, market pair
The demand of natural is significantly increased.And natural extraction cost is higher and inevitably there is impurity,
Cause purity lower, and due to mostly playing a role using monomeric form as effective component, is not only easy to be metabolized, but also antioxygen
It is lower to change activity.
In consideration of it, the present invention proposes that a kind of antioxidant, the antioxidant include esterification rice bran polysaccharide.
Rice bran polysaccharide is present in the caryopsis cortex of paddy, is primarily referred to as molecular weight not equal a kind of non-starch polysaccharide, tool
There is the function of removing hydroxyl radical free radical, but as most of naturals, also has unstable, degradable and anti-oxidant
The lower defect of activity.After carrying out esterification modification to rice bran polysaccharide, modified outcome still has an anti-oxidation function, or even due to
Synergistic effect can play effect more stronger than monomer when playing antioxidation, and be esterified modified outcome as rice
The derivative substance of chaff polysaccharide, property are stablized, are easy to be absorbed by organisms and have no toxic side effect to body.In addition, China's rice bran produces
Amount is extremely abundant, and for the present invention to be esterified rice bran polysaccharide as antioxidant, raw material sources are huge and cheap, reduce well
Antioxidant cost, develops and is utilized this precious resources of rice bran, the direction that has been the application extension of rice bran.
In addition, to solve the above problems, the invention also provides a kind of preparation methods of antioxidant, as shown in connection with fig. 1
Antioxidant preparation method an embodiment flow diagram, the preparation method of the antioxidant includes following step
It is rapid:
Step S10, chlorosulfonic acid is added dropwise into anhydrous pyridine, reaction forms esterifying reagent.
When step S10 is implemented, in one embodiment of the invention, step S10 may include:
Reaction vessel equipped with anhydrous pyridine is placed in ice salt bath cooling；
Under ice salt bath, chlorosulfonic acid is slowly added dropwise into the reaction vessel while stirring, reaction forms esterifying reagent.
Wherein, the volume ratio of the chlorosulfonic acid and anhydrous pyridine is 1:(3~5)；The temperature when reaction is 0~4 DEG C,
The time of the reaction is 0.5~2h.
Pyridine can generate pyridine-sulfotrioxide compound when mixing with chlorosulfonic acid, this is a kind of higher ester of reactivity
Change reagent, can be used for being esterified modification.Vigorous reaction can be occurred by meeting water due to chlorosulfonic acid, in the process for preparing esterifying reagent
In, need the moisture in strict control system, so, the present invention selects anhydrous pyridine, and using at low temperature, by chlorosulfonic acid by
The mode of operation being added dropwise in anhydrous pyridine.Meanwhile to guarantee that smoothly, safely forward direction carries out for reaction, whole mistakes of step S10
Cheng Junying is carried out at cryogenic conditions, preferably 0~4 DEG C, to guarantee that this temperature environment, the present invention are preferably ice salt bath, phase
For ice-water bath, temperature can be adjusted to lower, and range of temperature is smaller.Adjust the ratio of pyridine and chlorosulfonic acid, it can
The esterifying reagent of different proportion is obtained, and then influences the degree of substitution and yield of esterification rice bran polysaccharide, in the present embodiment, chlorosulfonic acid
Volume ratio with anhydrous pyridine is 1:(3~5), preferably 1:4.
Step S20, rice bran polysaccharide, stirring to formation suspension system are added into n,N-Dimethylformamide.
Step S30, the esterifying reagent is added in the suspension system, stirring forms reaction solution.
Wherein, the solid-to-liquid ratio (g:L) of the rice bran polysaccharide in the suspension system and the esterifying reagent is (5~7): 1；Institute
When stating to form reaction solution, reaction temperature is 60~80 DEG C, and the reaction time is 1.5~2h.
It is hardened to prevent when mixing esterifying reagent and rice bran polysaccharide, rice bran polysaccharide first can be suspended in N,
In dinethylformamide, in this way when esterifying reagent to be added in suspension system, n,N-Dimethylformamide can be played
The effect of hydrotropy, rice bran polysaccharide are easier to be esterified.Due to the proportion of the proportion of esterifying reagent, esterifying reagent and rice bran polysaccharide, with
And reaction temperature and time can all influence the yield of reaction and the degree of substitution of sulfate, and degree of substitution can direct shadow
The bioactivity to esterification rice bran polysaccharide is rung, therefore, it is necessary to select suitable reaction condition, in the present embodiment, the suspension
The solid-to-liquid ratio (g:L) of rice bran polysaccharide and the esterifying reagent in system is preferably (5~7): 1；When the formation reaction solution,
Reaction temperature is preferably 60~80 DEG C, and the reaction time is preferably 1.5~2h.
Step S40, after the adjusting reaction solution is in neutrality, consolidated after 95% ethyl alcohol is added in Xiang Suoshu reaction solution
Liquid separation, must precipitate.
When step S40 is implemented, in another embodiment of the present invention, step S40 may include:
The pH that sodium hydroxide solution is added dropwise to the reaction solution into the reaction solution is 6.8~7.2, is obtained neutral molten
Liquid；
Then 95% ethyl alcohol is added into the neutral solution and forms mixed solution, when ethyl alcohol is in the mixed solution
When mass fraction is 70%, stop that 95% ethyl alcohol is added；
The mixed solution is centrifuged, must be precipitated.
Wherein, the concentration of sodium hydroxide solution is 1~5mol/L.
Since rice bran polysaccharide and esterifying reagent meet alkali soluble solution, to avoid local hydrolysis, sodium hydroxide solution is being added
When need be added dropwise.Simultaneously as esterification rice bran polysaccharide different solubility in the ethyl alcohol of different quality containing, passes through alcohol
It washes, can be precipitated.
Step S50, it dialyses after taking the precipitating to be dissolved in water, collects and retain liquid vacuum concentration, rice must be esterified after dry
Chaff polysaccharide.
Wherein, the dialyzate used of dialysing is water；The dialysis time is 24~48h.
In precipitating in addition to being esterified rice bran polysaccharide, also contains some impurity, is dialysed, impurity can be removed by distilled water,
Improve the purity that rice bran polysaccharide is esterified in final product.
It is more more stable than the property of rice bran polysaccharide to be esterified rice bran polysaccharide, and there is stronger anti-oxidation function, and due to sulphur
Acidification, water solubility enhancing, is easily absorbed by organisms and has no toxic side effect to body.To be esterified rice bran polysaccharide as anti-oxidant
Agent, it is low in cost, and be the application extension of rice bran direction.
Technical solution of the present invention is described in further detail below in conjunction with specific embodiments and the drawings, it should be understood that
Following embodiment is only used to explain the present invention, is not intended to limit the present invention.
Embodiment 1
Cooling anhydrous pyridine will be pre-placed in refrigerator to be placed in in the three-necked bottle of condenser pipe and agitating device, with
Ice salt bath is cooling；It is 1:4 (20ml:80ml) slow according to the volume ratio of chlorosulfonic acid and anhydrous pyridine under the state that is vigorously stirred
Chlorosulfonic acid is added dropwise, continues ice salt bath cooling, makes reaction temperature control at 4 DEG C, obtains flaxen esterifying reagent after reacting 1h.
It accurately weighs the rice bran polysaccharide of 500mg and is suspended in 35ml n,N-Dimethylformamide (DMF), is added
Prepared above-mentioned esterifying reagent 100ml, is stirred to react 2h at 70 DEG C.
To which after reaction, being neutralized to pH value with the titration of 4mol/L NaOH solution is 6.8.To the neutral solution after neutralization
95% ethyl alcohol of middle addition forms mixed solution, until ethyl alcohol mass fraction is 70% in mixed solution.By mixed solution centrifugation point
From taking precipitating.
Precipitating is dissolved in distilled water, for 24 hours with distilled water dialysis, collects and retains liquid vacuum concentration, rice must be esterified after dry
Chaff polysaccharide.
Embodiment 2
Cooling anhydrous pyridine will be pre-placed in refrigerator to be placed in in the three-necked bottle of condenser pipe and agitating device, with
Ice salt bath is cooling；It is 1:3 (20ml:60ml) slow according to the volume ratio of chlorosulfonic acid and anhydrous pyridine under the state that is vigorously stirred
Chlorosulfonic acid is added dropwise, continues ice salt bath cooling, makes reaction temperature control at 2 DEG C, obtains flaxen esterifying reagent after reacting 0.5h.
It accurately weighs the rice bran polysaccharide of 350mg and is suspended in 35ml n,N-Dimethylformamide (DMF), is added
Prepared above-mentioned esterifying reagent 50ml, is stirred to react 1.5h at 60 DEG C.
To which after reaction, being neutralized to pH value with the titration of 1mol/L NaOH solution is 7.2.To the neutral solution after neutralization
95% ethyl alcohol of middle addition forms mixed solution, until ethyl alcohol mass fraction is 70% in mixed solution.By mixed solution centrifugation point
From taking precipitating.
Precipitating is dissolved in distilled water, with distilled water dialysis 48h, collects and retains liquid vacuum concentration, rice must be esterified after dry
Chaff polysaccharide.
Embodiment 3
Cooling anhydrous pyridine will be pre-placed in refrigerator to be placed in in the three-necked bottle of condenser pipe and agitating device, with
Ice salt bath is cooling；It is 1:5 (20ml:100ml) slow according to the volume ratio of chlorosulfonic acid and anhydrous pyridine under the state that is vigorously stirred
Chlorosulfonic acid is added dropwise, continues ice salt bath cooling, makes reaction temperature control at 0 DEG C, obtains flaxen esterifying reagent after reacting 2h.
It accurately weighs the rice bran polysaccharide of 650mg and is suspended in 35ml n,N-Dimethylformamide (DMF), is added
Prepared above-mentioned esterifying reagent 100ml, is stirred to react 1.8h at 75 DEG C.
To which after reaction, being neutralized to pH value with the titration of 5mol/L NaOH solution is 7.0.To the neutral solution after neutralization
95% ethyl alcohol of middle addition forms mixed solution, until ethyl alcohol mass fraction is 70% in mixed solution.By mixed solution centrifugation point
From taking precipitating.
Precipitating is dissolved in distilled water, with distilled water dialysis 30h, collects and retains liquid vacuum concentration, it is more to obtain rice bran after dry
The sulphation modification product of sugar.
Embodiment 4
Cooling anhydrous pyridine will be pre-placed in refrigerator to be placed in in the three-necked bottle of condenser pipe and agitating device, with
Ice salt bath is cooling；It is 1:4 (20ml:80ml) slow according to the volume ratio of chlorosulfonic acid and anhydrous pyridine under the state that is vigorously stirred
Chlorosulfonic acid is added dropwise, continues ice salt bath cooling, makes reaction temperature control at 1 DEG C, obtains flaxen esterifying reagent after reacting 1.2h.
It accurately weighs the rice bran polysaccharide of 600mg and is suspended in 35ml n,N-Dimethylformamide (DMF), is added
Prepared above-mentioned esterifying reagent 100ml, is stirred to react 1.8h at 68 DEG C.
To which after reaction, being neutralized to pH value with the titration of 2mol/L NaOH solution is 6.9.To the neutral solution after neutralization
95% ethyl alcohol of middle addition forms mixed solution, until ethyl alcohol mass fraction is 70% in mixed solution.By mixed solution centrifugation point
From taking precipitating.
Precipitating is dissolved in distilled water, with distilled water dialysis 36h, collects and retains liquid vacuum concentration, rice must be esterified after dry
Chaff polysaccharide.
Embodiment 5
Cooling anhydrous pyridine will be pre-placed in refrigerator to be placed in in the three-necked bottle of condenser pipe and agitating device, with
Ice salt bath is cooling；It is 1:4 (20ml:80ml) slow according to the volume ratio of chlorosulfonic acid and anhydrous pyridine under the state that is vigorously stirred
Chlorosulfonic acid is added dropwise, continues ice salt bath cooling, makes reaction temperature control at 4 DEG C, obtains flaxen esterifying reagent after reacting 1.5h.
It accurately weighs the rice bran polysaccharide of 550mg and is suspended in 35ml n,N-Dimethylformamide (DMF), is added
Prepared above-mentioned esterifying reagent 100ml, is stirred to react 2h at 70 DEG C.
To which after reaction, being neutralized to pH value with the titration of 4mol/L NaOH solution is 7.Into the neutral solution after neutralization
95% ethyl alcohol is added and forms mixed solution, until ethyl alcohol mass fraction is 70% in mixed solution.Mixed solution is centrifugated,
Take precipitating.
Precipitating is dissolved in distilled water, with distilled water dialysis 44h, collects and retains liquid vacuum concentration, rice must be esterified after dry
Chaff polysaccharide.
Embodiment 6
Cooling anhydrous pyridine will be pre-placed in refrigerator to be placed in in the three-necked bottle of condenser pipe and agitating device, with
Ice salt bath is cooling；It is 1:4 (20ml:80ml) slow according to the volume ratio of chlorosulfonic acid and anhydrous pyridine under the state that is vigorously stirred
Chlorosulfonic acid is added dropwise, continues ice salt bath cooling, makes reaction temperature control at 4 DEG C, obtains flaxen esterifying reagent after reacting 0.8h.
It accurately weighs the rice bran polysaccharide of 600mg and is suspended in 35ml n,N-Dimethylformamide (DMF), is added
Prepared above-mentioned esterifying reagent 100ml, is stirred to react 2h at 73 DEG C.
To which after reaction, being neutralized to pH value with the titration of 3mol/L NaOH solution is 7.Into the neutral solution after neutralization
95% ethyl alcohol is added and forms mixed solution, until ethyl alcohol mass fraction is 70% in mixed solution.Mixed solution is centrifugated,
Take precipitating.
Precipitating is dissolved in distilled water, with distilled water dialysis 46h, collects and retains liquid vacuum concentration, rice must be esterified after dry
Chaff polysaccharide.
Scavenging action to hydroxyl free radical compliance test result is carried out by phenanthroline method to product made from Examples 1 to 6.
Be added into phenanthroline-Fenton system it is a certain amount of (50uL, 100uL, 150uL, 200uL, 250uL, 300uL,
350uL, 400uL) esterification rice bran polysaccharide, with ultraviolet specrophotometer measure absorbance, be denoted as Ax, Examples 1 to 6 preparation
Antioxidant and rice bran polysaccharide detect according to the above method.The control group measurement absorbance that esterification rice bran polysaccharide is not added is denoted as A；
The absorbance of blank control system is denoted as A0。
The clearance rate to OH free radical is calculated according to the following formula and to draw line chart as shown in Figure 2.
Formula: OH free radical scavenging activity (%)=[(Ax-A)/(A0-A)]×100
In Fig. 2, A is the change curve of Scavenging action to hydroxyl free radical after the rice bran polysaccharide of various concentration is added；
B is the change curve of Scavenging action to hydroxyl free radical after 1 product of embodiment of various concentration is added；
C is the change curve of Scavenging action to hydroxyl free radical after 2 product of embodiment of various concentration is added；
D is the change curve of Scavenging action to hydroxyl free radical after 3 product of embodiment of various concentration is added；
E is the change curve of Scavenging action to hydroxyl free radical after 4 product of embodiment of various concentration is added；
F is the change curve of Scavenging action to hydroxyl free radical after 5 product of embodiment of various concentration is added；
G is the change curve of Scavenging action to hydroxyl free radical after 6 product of embodiment of various concentration is added.
As shown in Figure 2, when sample-adding amount is less than 150 μ L, scavenging effect and rice bran of the rice bran polysaccharide to hydroxy radical are esterified
Polysaccharide is suitable；When sample-adding amount is greater than 150 μ L, it is more that rice bran is significantly greater than to the scavenging effect esterification rice bran polysaccharide of hydroxy radical
Sugar.All in all, rice bran polysaccharide enhances Hydroxyl Radical Scavenging after over-churning is modified, and is used according to normal health care product
It is more advantageous that rice bran polysaccharide is esterified for amount.
The above is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, for this field
For technical staff, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any
Modification, equivalent replacement, improvement etc. should all be included within the scope of the present invention.
Claims (10)
1. a kind of antioxidant, which is characterized in that including being esterified rice bran polysaccharide.
2. a kind of preparation method of antioxidant as described in claim 1, which comprises the following steps:
Chlorosulfonic acid is added dropwise into anhydrous pyridine, reaction forms esterifying reagent；
Rice bran polysaccharide, stirring to formation suspension system are added into n,N-Dimethylformamide；
The esterifying reagent is added in the suspension system, stirring forms reaction solution；
It adjusts after the reaction solution is in neutrality, is separated by solid-liquid separation after 95% ethyl alcohol is added in Xiang Suoshu reaction solution, it is heavy to obtain
It forms sediment；
It dialyses after taking the precipitating to be dissolved in water, collects and retain liquid vacuum concentration, rice bran polysaccharide must be esterified after dry.
3. the preparation method of antioxidant as claimed in claim 2, which is characterized in that described that chlorine sulphur is added dropwise into anhydrous pyridine
The step of acid, reaction forms esterifying reagent, comprising:
Reaction vessel equipped with anhydrous pyridine is placed in ice salt bath cooling；
Under ice salt bath, chlorosulfonic acid is slowly added dropwise into the reaction vessel while stirring, reaction forms esterifying reagent；
Wherein, the volume ratio of the chlorosulfonic acid and anhydrous pyridine is 1:(3~5).
4. the preparation method of antioxidant as claimed in claim 3, which is characterized in that it is described under ice salt bath, while stirring
It is slowly added dropwise chlorosulfonic acid into the reaction vessel, in the step of reaction forms esterifying reagent, the temperature when reaction is 0~
4 DEG C, the time of the reaction is 0.5~2h.
5. the preparation method of antioxidant as claimed in claim 2, which is characterized in that described that the esterifying reagent is added to institute
In the step of stating in suspension system, forming reaction solution, rice bran polysaccharide in the suspension system is consolidated with the esterifying reagent
Liquor ratio (g:L) is (5~7): 1.
6. the preparation method of antioxidant as claimed in claim 2, which is characterized in that described that the esterifying reagent is added to institute
It states in suspension system, in stirring the step of forming reaction solution, when the is formationed reaction solution, reaction temperature is 60~80 DEG C,
The reaction time is 1.5~2h.
7. the preparation method of antioxidant as claimed in claim 2, which is characterized in that described to adjust during the reaction solution is in
After property, the step of be separated by solid-liquid separation after 95% ethyl alcohol is added in Xiang Suoshu reaction solution, obtain precipitating, comprising:
The pH that sodium hydroxide solution is added dropwise to the reaction solution into the reaction solution is 6.8~7.2, obtains neutral solution；
Then 95% ethyl alcohol is added into the neutral solution and forms mixed solution, when quality of the ethyl alcohol in the mixed solution
When score is 70%, stop that 95% ethyl alcohol is added；
The mixed solution is centrifuged, must be precipitated.
8. the preparation method of antioxidant as claimed in claim 7, which is characterized in that described to be added dropwise into the reaction solution
In the step of pH of sodium hydroxide solution to the reaction solution is 6.8~7.2, obtains neutral solution, the sodium hydroxide solution
Concentration be 1~5mol/L.
9. the preparation method of antioxidant as claimed in claim 2, which is characterized in that described to take the precipitating to be dissolved in water laggard
In the step of row dialysis collects and retains liquid vacuum concentration, must be esterified rice bran polysaccharide after dry, dialyzate that the dialysis uses for
Water.
10. the preparation method of antioxidant as claimed in claim 2, which is characterized in that it is described take it is described precipitating be dissolved in water after
In the step of dialysing, collecting and retain liquid vacuum concentration, rice bran polysaccharide must be esterified after dry,
The dialysis time is 24~48h.
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