CN108976310A - A kind of preparation method of radix tetrastigme zinc polysaccharide anti-oxidative agent - Google Patents
A kind of preparation method of radix tetrastigme zinc polysaccharide anti-oxidative agent Download PDFInfo
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- CN108976310A CN108976310A CN201810883007.0A CN201810883007A CN108976310A CN 108976310 A CN108976310 A CN 108976310A CN 201810883007 A CN201810883007 A CN 201810883007A CN 108976310 A CN108976310 A CN 108976310A
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- C—CHEMISTRY; METALLURGY
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
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- A61P39/06—Free radical scavengers or antioxidants
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The invention discloses a kind of preparation methods of radix tetrastigme zinc polysaccharide anti-oxidative agent, prepare radix tetrastigme polysaccharide first and are configured to certain density solution.The zinc source is zinc sulfate, zinc chloride or zinc acetate, certain concentration solution is made into be added in radix tetrastigme polysaccharide solution, sodium hydroxide solution is added in toward reaction system and controls reaction system pH, control reaction temperature and agitating solution after a certain period of time, centrifugation collects supernatant and is cleaned with bag filter dialysis, is finally freeze-dried to obtain radix tetrastigme zinc polysaccharide anti-oxidative agent to solution.Radix tetrastigme zinc polysaccharide anti-oxidative agent of the invention is while improving body antioxygenic property, zinc supplementation agent can also be used as, maintain body normal physiological function, also containing the active material polysaccharide extracted in radix tetrastigme in product, with clearing heat and detoxicating, heat dissipation tonifying spleen and other effects, has certain medical value and application prospect.
Description
Technical field
The present invention relates to antioxidant preparation fields, and in particular to a kind of preparation side of radix tetrastigme zinc polysaccharide anti-oxidative agent
Method.
Background technique
Radix tetrastigme, rectify name tetratigma hemsleyanum also known as hemsley rockvine root, gold thread hoist, Vitaceae herbaceous species.Herb can enter
Medicine.Mainly it is grown in the areas such as Zhejiang, Hunan, Jiangxi, Fujian, Hubei, Guangdong, Guangxi, Sichuan.With clearing heat and detoxicating, wind-dispelling
Resolving sputum, promoting blood circulation and stopping pain and other effects have good medical value.
Zn-ef ficiency is microelement necessary to maintaining body normal physiological function and biochemical metabolism, and zinc is sent out in growth in humans
It educates, play an important role in reproduction heredity, the important physiology course such as immune, endocrine.
Zn-ef ficiency is found to have many important function, it can promote growth in humans to develop, and maintains human normal appetite,
Promote wound healing, maintain the normal sperm function of male, improve resistance, improves glycometabolism etc..
Antioxidant, which refers to, can prevent or delay Food Oxidation, improve the stability of food and extend the food additive of storage period
Add agent.The proper use of storage period that can not only extend food of antioxidant, shelf life bring good to the producer, consumer
Good economic benefit, and better food safety is brought to consumer.
Therefore, a kind of food antioxidant is researched and developed, makes it not only and have the function of to improve body antioxygenic property, and can be with
As zinc supplementation agent, have great importance.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of radix tetrastigme zinc polysaccharide anti-oxidative agent.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of radix tetrastigme zinc polysaccharide anti-oxidative agent comprising following steps:
(1) by radix tetrastigme pre-treatment:
It takes radix tetrastigme ground position to clean, dries, crush；
(2) radix tetrastigme Polyose extraction:
Using the hot water extraction radix tetrastigme powder a few hours of certain temperature, filtrate is collected, and certain volume chlorine is added in filtrate
Imitative and n-butanol is stirred, and is then centrifuged for removing albumin layer and organic layer, residual filtrate is dialysed to system organic solvent-free
After be freeze-dried to obtain radix tetrastigme polysaccharide；
(3) the polysaccharide anti-oxidative agent of radix tetrastigme zinc is prepared:
Radix tetrastigme polysaccharide is configured to certain density radix tetrastigme polysaccharide solution, certain density zinc source solution, institute is then added
Stating zinc source is zinc sulfate, zinc chloride or zinc acetate, and the radix tetrastigme polysaccharide and zinc source mass ratio are 1:1-1:5, then will be anti-
System is answered to be placed in 40-90 DEG C of stirring；
Whipping process controls the pH value of reaction system in 5-12, reacts and continue 60- toward sodium hydroxide solution is added in reaction system
300min；
After reaction, centrifuging and taking supernatant dialyses supernatant with bag filter, collects solution and is freeze-dried, obtains three
Leaf blueness zinc polysaccharide anti-oxidative agent.
Step (2) the hot water extraction condition are as follows: 40 ~ 90 DEG C of temperature, the time is 3 ~ 8h, and solid-liquid ratio is 1:10 ~ 1:50 g/
mL。
The volume ratio of chloroform and n-butanol that the step (2) is added is 3:1-6:1.
The concentration that step (3) the radix tetrastigme polysaccharide is prepared is 1 ~ 20mg/ml, in the solution of zinc source zinc ion concentration be 1 ~
20mg/ml, naoh concentration 1mol/L, reaction pH are 5-12, react and continue 60-300min.
The invention adopts the above technical scheme, from radix tetrastigme overground part extract active Chinese drug component substance polysaccharide, and with zinc source (sulphur
Sour zinc, zinc chloride, zinc acetate) reaction, radix tetrastigme zinc polysaccharide anti-oxidative agent is prepared.The radix tetrastigme zinc that the present invention is prepared
Polysaccharide anti-oxidative agent is also used as zinc supplementation agent while improving antioxidant ability of organism, maintains the normal physiological function of body
Can, Zn content is 20mg/g or so.In addition, being greatly improved in product containing the active material polysaccharide extracted in radix tetrastigme
Original pharmacological activity, for example have a higher oxidation resistance etc..Radix tetrastigme zinc polysaccharide anti-oxidative prepared by the present invention
The oxidation resistance of agent is higher by 30% or so than the radix tetrastigme polysaccharide of same concentration.
Specific embodiment
A kind of preparation method of radix tetrastigme zinc polysaccharide anti-oxidative agent, comprising the following steps:
(1) by radix tetrastigme pre-treatment:
It takes radix tetrastigme significant points to clean, dries, crush；
Wherein, materials position is the ground position of radix tetrastigme.
(2) radix tetrastigme Polyose extraction:
It is 1:10 ~ 1:50 g/mL by solid-liquid ratio using the hot water of 40 ~ 90 DEG C of temperature, after extracting 3 ~ 8h of radix tetrastigme powder, collects
Filtrate, and in filtrate be added 3:1-6:1 volume ratio chloroform and n-butanol be stirred, be then centrifuged for remove albumin layer and
Organic layer is freeze-dried to obtain radix tetrastigme polysaccharide after residual filtrate is dialysed to system organic solvent-free；
(3) the polysaccharide anti-oxidative agent of radix tetrastigme zinc is prepared:
Radix tetrastigme polysaccharide is configured to the radix tetrastigme polysaccharide solution of 1 ~ 20mg/ml concentration, the zinc of 1 ~ 20mg/ml concentration is then added
Source, the zinc source are zinc sulfate, zinc chloride or zinc acetate, and the radix tetrastigme polysaccharide and zinc source mass ratio are 1:1-1:5, then
Reaction system is placed in 40-90 DEG C of stirring；
Whipping process controls the pH value of reaction system in 5-12, reaction toward addition 1mol/L sodium hydroxide solution in reaction system
Continue 60-300min；
After reaction, centrifuging and taking supernatant dialyses supernatant with bag filter, collects solution and is freeze-dried, obtains three
Leaf blueness zinc polysaccharide anti-oxidative agent.
The test of DPPH free radical scavenging ability:
Free radical is configured to 1.3 × 10 with dehydrated alcohol-3The mother liquor of mol/L dilutes 20 times with dehydrated alcohol when use, dense
Degree is 65 μm of ol/L.2mL sample solution is taken, 65 μm of ol/L free radical ethanol solution 2mL are added, is protected from light stands 30min at room temperature
Afterwards, absorbance is surveyed at 517nm.
DPPH free radical scavenging activity calculates as follows:
Clearance rate=[1- (Ai-Aj)/A0]×100%
A in formula0The light absorption value of -2.0mL free-atom aqueous solution+2.0mL dehydrated alcohol;
AiThe light absorption value of -2.0mL DPPH free-atom aqueous solution sample liquid;
The light absorption value of Aj-2.0mL dehydrated alcohol+2.0mL sample liquid.
DPPH free radical scavenging activity is bigger, shows that oxidation resistance is stronger.
Embodiment 1
A kind of preparation method of radix tetrastigme zinc polysaccharide anti-oxidative agent, comprising the following steps:
(1) by radix tetrastigme pre-treatment:
It takes radix tetrastigme significant points to clean, dries, crush；
Wherein, materials position is the ground position of radix tetrastigme.
(2) radix tetrastigme Polyose extraction:
It is 1:10g/mL by solid-liquid ratio using the hot water of 40 DEG C of temperature, after extracting radix tetrastigme powder 3h, collects filtrate, and filtering
The chloroform of 6:1 volume ratio is added in liquid and n-butanol is stirred, is then centrifuged for removing albumin layer and organic layer, residue is filtered
Liquid is freeze-dried to obtain radix tetrastigme polysaccharide after dialysing to system organic solvent-free；
(3) the polysaccharide anti-oxidative agent of radix tetrastigme zinc is prepared:
Radix tetrastigme polysaccharide is configured to the radix tetrastigme polysaccharide solution of 5mg/ml concentration, the zinc source of 20mg/ml concentration, institute is then added
Stating zinc source is zinc sulfate, and the radix tetrastigme polysaccharide and zinc source mass ratio are 1:5, and reaction system is then placed in 90 DEG C of stirrings；
Whipping process controls the pH value of reaction system 12, reaction is held toward addition 1mol/L sodium hydroxide solution in reaction system
Continuous 100min；
After reaction, centrifuging and taking supernatant dialyses supernatant with bag filter, collects solution and is freeze-dried, obtains three
Leaf blueness zinc polysaccharide anti-oxidative agent.
Radix tetrastigme zinc polysaccharide anti-oxidative agent manufactured in the present embodiment, Zn content 20mg/g.
Embodiment 2
A kind of preparation method of radix tetrastigme zinc polysaccharide anti-oxidative agent, comprising the following steps:
(1) by radix tetrastigme pre-treatment:
It takes radix tetrastigme significant points to clean, dries, crush；
Wherein, materials position is the ground position of radix tetrastigme.
(2) radix tetrastigme Polyose extraction:
It is 1:30 g/mL by solid-liquid ratio using the hot water of 60 DEG C of temperature, after extracting radix tetrastigme powder 5h, collects filtrate, and filtering
The chloroform of 4:1 volume ratio is added in liquid and n-butanol is stirred, is then centrifuged for removing albumin layer and organic layer, residue is filtered
Liquid is freeze-dried to obtain radix tetrastigme polysaccharide after dialysing to system organic solvent-free；
(3) the polysaccharide anti-oxidative agent of radix tetrastigme zinc is prepared:
Radix tetrastigme polysaccharide is configured to the radix tetrastigme polysaccharide solution of 1mg/ml concentration, the zinc source of 10mg/ml concentration, institute is then added
Stating zinc source is zinc chloride, and the radix tetrastigme polysaccharide and zinc source mass ratio are 1:3, and reaction system is then placed in 70 DEG C of stirrings；
Whipping process controls the pH value of reaction system 7, reaction continues toward addition 1mol/L sodium hydroxide solution in reaction system
60min；
After reaction, centrifuging and taking supernatant dialyses supernatant with bag filter, collects solution and is freeze-dried, obtains three
Leaf blueness zinc polysaccharide anti-oxidative agent.
Radix tetrastigme zinc polysaccharide anti-oxidative agent manufactured in the present embodiment, Zn content 17mg/g.
Embodiment 3
A kind of preparation method of radix tetrastigme zinc polysaccharide anti-oxidative agent, comprising the following steps:
(1) by radix tetrastigme pre-treatment:
It takes radix tetrastigme significant points to clean, dries, crush；
Wherein, materials position is the ground position of radix tetrastigme.
(2) radix tetrastigme Polyose extraction:
It is 1:50 g/mL by solid-liquid ratio using the hot water of 90 DEG C of temperature, after extracting radix tetrastigme powder 8h, collects filtrate, and filtering
The chloroform of 3:1 volume ratio is added in liquid and n-butanol is stirred, is then centrifuged for removing albumin layer and organic layer, residue is filtered
Liquid is freeze-dried to obtain radix tetrastigme polysaccharide after dialysing to system organic solvent-free；
(3) the polysaccharide anti-oxidative agent of radix tetrastigme zinc is prepared:
Radix tetrastigme polysaccharide is configured to the radix tetrastigme polysaccharide solution of 20mg/ml concentration, the zinc source of 1mg/ml concentration, institute is then added
Stating zinc source is zinc acetate, and the radix tetrastigme polysaccharide and zinc source mass ratio are 1:1, and reaction system is then placed in 40 DEG C of stirrings；
Whipping process controls the pH value of reaction system 5, reaction continues toward addition 1mol/L sodium hydroxide solution in reaction system
300min；
After reaction, centrifuging and taking supernatant dialyses supernatant with bag filter, collects solution and is freeze-dried, obtains three
Leaf blueness zinc polysaccharide anti-oxidative agent.
Radix tetrastigme zinc polysaccharide anti-oxidative agent manufactured in the present embodiment, Zn content 33mg/g.
Radix tetrastigme zinc polysaccharide anti-oxidative agent prepared by the present embodiment 1-3 and vitamin carry out free radical scavenging ability survey
Examination.To the IC of free radical50When value refers to that free radical scavenging activity reaches, the concentration of reducing agent used.
1 oxidation resistance test result of table
Free radical scavenging ability test result shows, the IC of vitamin50Value is 1.55, the IC of radix tetrastigme polysaccharide50Value is 1.87.
The IC of the radix tetrastigme zinc polysaccharide anti-oxidative agent of the present embodiment 150Value is 0.43, is 0.27 or so of vitamin, is radix tetrastigme polysaccharide
0.23 times.The IC of the radix tetrastigme zinc polysaccharide anti-oxidative agent of the present embodiment 250Value is 0.57, is the 0.36 of vitamin, is radix tetrastigme
0.3 times of polysaccharide.The IC of the radix tetrastigme zinc polysaccharide anti-oxidative agent of the present embodiment 350Value is 0.39, is the 0.25 of vitamin, is three
0.2 times of leaf blueness polysaccharide.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (6)
1. a kind of preparation method of radix tetrastigme zinc polysaccharide anti-oxidative agent, it is characterised in that: the following steps are included:
(1) radix tetrastigme pre-treatment:
It takes the ground position of radix tetrastigme to be washed, dries, crush；
(2) radix tetrastigme Polyose extraction:
Using hot water extraction radix tetrastigme powder, collect filtrate, and chloroform be added in filtrate and n-butanol is stirred, then from
The heart removes albumin layer and organic layer, and radix tetrastigme polysaccharide is freeze-dried to obtain after residual filtrate is dialysed to system organic solvent-free；
(3) the polysaccharide anti-oxidative agent of radix tetrastigme zinc is prepared:
Radix tetrastigme polysaccharide is configured to radix tetrastigme polysaccharide solution, zinc source solution is then added, the zinc source is zinc sulfate, zinc chloride
Or zinc acetate, the radix tetrastigme polysaccharide and zinc source mass ratio are 1:1-1:5, and reaction system is then placed in 40-90 DEG C of stirring；
Whipping process controls the pH value of reaction system in 5-12, reacts and continue 60- toward sodium hydroxide solution is added in reaction system
300min；
After reaction, centrifuging and taking supernatant dialyses supernatant with bag filter, collects solution and is freeze-dried, obtains three
Leaf blueness zinc polysaccharide anti-oxidative agent.
2. a kind of preparation method of radix tetrastigme zinc polysaccharide anti-oxidative agent according to claim 1, it is characterised in that: step
(2) hot water extraction condition are as follows: 40 ~ 90 DEG C of temperature, the time is 3 ~ 8h, and solid-liquid ratio is 1:10 ~ 1:50 g/mL.
3. a kind of preparation method of radix tetrastigme zinc polysaccharide anti-oxidative agent according to claim 1, it is characterised in that: step
(2) volume ratio of the chloroform and n-butanol that are added is 3:1-6:1.
4. a kind of preparation method of radix tetrastigme zinc polysaccharide anti-oxidative agent according to claim 1, it is characterised in that: step
(3) concentration that radix tetrastigme polysaccharide is prepared is 1 ~ 20mg/ml.
5. a kind of preparation method of radix tetrastigme zinc polysaccharide anti-oxidative agent according to claim 1, it is characterised in that: step
(3) zinc ion concentration is 1 ~ 20mg/ml in zinc source solution.
6. a kind of preparation method of radix tetrastigme zinc polysaccharide anti-oxidative agent according to claim 1, it is characterised in that: step
(3) naoh concentration is 1mol/L.
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Cited By (3)
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| CN110330574A (en) * | 2019-07-08 | 2019-10-15 | 武汉轻工大学 | The preparation method and zinc supplementation agent of polysaccharide zinc complexes |
| CN112048025A (en) * | 2020-08-31 | 2020-12-08 | 华南理工大学 | Zinc supplement water-soluble soybean polysaccharide zinc chelate as well as preparation method and application thereof |
| CN114521570A (en) * | 2022-01-17 | 2022-05-24 | 郑州轻工业大学 | Lentinan antibacterial compound and preparation method thereof |
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| CN112048025A (en) * | 2020-08-31 | 2020-12-08 | 华南理工大学 | Zinc supplement water-soluble soybean polysaccharide zinc chelate as well as preparation method and application thereof |
| CN114521570A (en) * | 2022-01-17 | 2022-05-24 | 郑州轻工业大学 | Lentinan antibacterial compound and preparation method thereof |
| CN114521570B (en) * | 2022-01-17 | 2023-04-25 | 郑州轻工业大学 | Lentinan antibacterial compound and preparation method thereof |
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Application publication date: 20181211 |