CN110078839A - It is a kind of to utilize magnetic mesoporous SiO2@Fe3O4Extract the preparation method of polysaccharide in Rumex madaio - Google Patents
It is a kind of to utilize magnetic mesoporous SiO2@Fe3O4Extract the preparation method of polysaccharide in Rumex madaio Download PDFInfo
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- CN110078839A CN110078839A CN201811604153.1A CN201811604153A CN110078839A CN 110078839 A CN110078839 A CN 110078839A CN 201811604153 A CN201811604153 A CN 201811604153A CN 110078839 A CN110078839 A CN 110078839A
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- C—CHEMISTRY; METALLURGY
- 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
It is a kind of to utilize magnetic mesoporous SiO2@Fe3O4The preparation method (1) for extracting polysaccharide in Rumex madaio cleans fresh Rumex madaio, then chooses root, root is placed in 50-70 ° of hothouse and is dried to constant-quality；(2) dry root is carried out using disintegrating machine being crushed to powder, is placed spare in bottle；(3) part Rhubarb is weighed, carries out microblogging ultrasonication after ethanol solution is added；After propose heating extraction to after tasteless plus water obtains Radix Et Rhizoma Rhei extract.
Description
Technical field:
This hair is related to a kind of magnetic mesoporous SiO of utilization2@Fe3O4The preparation method for extracting polysaccharide in Rumex madaio, belongs to organic matter system
Make technical field.
Background technique
Rumex madaio is called careless, invaluable, the wild wormwood artemisia Mai that spits blood, medicine dizzy greatly, lotus covered with gold leaf, aleppo dock rhizome etc., is a kind of root of plant
Pastern position, its medical value is very high, can play clearing heat and detoxicating, defaecation, desinsection, for equally having in the treatment of eczema very
Good effect.Rumex madaio root and rhizome is containing combining and free rheum emodin, Physcion, its total amount of rheum officinale amphyl are
1.14%, wherein mating type 0.87%, sequestered 0.27% also contain rumicin and a large amount of tannins.Also containing 6-O- the third two in root
Acyl-beta-methyl-D-glucopyranose glucoside and A Sikao bars of drawing acid.
We have found after studying prior art technology, Jie extracted currently without the polysaccharide to Rumex madaio
It continues.The only purifying technique of other chemical analysis of Rumex madaio.Wherein, number of patent application is a kind of entitled " quickly preparation
The method of high-purity Rumex madaio rheum emodin and deoxidation chrysaron ", due to being limited by equipment and technique, can only prepare every time several
Hundred milligrams of sample is far from satisfying the needs of new drug research and production.Wherein, number of patent application is, entitled
" the general method of Rumex madaio is extracted from Rheum hotaoense C. Y. Cheng et C. T. Kao " is extracted in preparation process, no using the inflammable and explosive organic solvent of low boiling point
But yield is low and is easy to happen safety accident, and is only prepared for a kind of general compound of Rumex madaio, and it is big not obtain deoxidation soil
Huang Pu results in waste of resources.Wherein, number of patent application is, entitled, and " it is big that a kind of high efficiency precisely isolates and purifies deoxidation soil
The method of Huang Pu ", due to needing by macroporous resin purification twice, technique is tediously long, and has to deoxygenate the general one kind of Rumex madaio
Compound, does not obtain that Rumex madaio is general, also results in the waste of resource.Wherein, number of patent application is " a kind of to separate Rumex madaio simultaneously
The Industrialized processing technique of glycosides and Rhapontin, deoxy- " it is isolated and purified using poly- phthalein amine, a large amount of solvent and energy consumption are needed, is separated
Solvent, which has, is unable to secondary recovery utilization, and environmental pollution is bigger.The present invention is on traditional microwave, ultrasonic technique, benefit
With Superparamagnetism mesoporous TiO2@Fe3O4The middle rheum emodin compound of Rumex madaio root is extracted, and application uniform design test is excellent
Change and extracts rheum emodin technique.
Summary of the invention:
To solve the above-mentioned problems, the present invention provides a kind of Superparamagnetism mesoporous SiO2@Fe3O4Nano particle can separate native big
The production technology of polysaccharide in Huang, the technique production procedure is simple, easy to operate, does not use poisonous and harmful solvent, only uses edible
Alcohol, SiO2@Fe3O4, can be with repeated recycling utilize with magnetism, but also have production cost low, product purity is high, is suitble to
In the industrialized production the features such as., energy consumption not only can be effectively reduced, and can thoroughly solve the problems, such as organic solvent residual, it is green
Color safety and environmental protection.
It utilizes magnetic mesoporous SiO2@Fe3O4Extract Rumex madaio in polysaccharide the preparation method comprises the following steps: the step is
(1) fresh Rumex madaio is cleaned, then chooses root, root is placed in 50-70 ° of hothouse and dried to constant
Quality；
(2) dry root is carried out using disintegrating machine being crushed to powder, is placed spare in bottle；
(3) part Rhubarb is weighed, carries out microblogging ultrasonication after ethanol solution is added；After propose heating extraction to after tasteless
Water is added to obtain Radix Et Rhizoma Rhei extract
(4) treated, and Radix Et Rhizoma Rhei extract measures absorbance, and the SiO of equivalent is added after measurement2@Fe3O4Nano particle, finally
To product.
As preferred: being placed on root in the step (1) in 65 ° of hothouse and dry to constant-quality.
As preferred: concentration is added into Rhubarb by the mass volume ratio of 1:1 to 1:20 in the step (3) is
The ethanol solution of 20%-95%, and heating and refluxing extraction 1-3 hours, extraction time is 1-3 times, and combined extract is concentrated into nothing
Taste adds water to obtain Radix Et Rhizoma Rhei extract,
As preferred: the magnetic mesoporous SiO2@Fe3O4The preparation method comprises the following steps: quasi- respectively with the electronic balance that precision is a ten thousandth
Really weigh 2.9-3.0gFeCl3·6H2The FeCl of O and 2.0-3.0g2·4H2O is placed in 250ml three-necked flask, in nitrogen atmosphere
Under, it is being 140-160g.l by 40-60ml concentration-1Aqueous Solutions of Polyethylene Glycol be added in above-mentioned beaker, heating water bath to 40-
60 °, under 900-1100rpm revolving speed, ammonium hydroxide is added, solution pH value adjustment is reacted into 30-40min between 10-12, uses magnetic
Iron is by Fe3O4Nanoparticle is separated with solvent, and Fe is washed with deionized3O4Nanoparticle, the Fe of washing3O4Nanoparticle
Son is placed in 250ml flask, by the SiO of 40-60ml concentration2Solution is added to the Fe after washing3O4In flask, will then it add
Enter deionized water to adjust the PH of mixed solution between 8-9, finally, ultrasonic disperse 10-20min obtains magnetic mesoporous SiO2@
Fe3O4Nanoparticle.
The present invention technique production procedure is simple, easy to operate, does not use poisonous and harmful solvent, only uses edible alcohol,
SiO2@Fe3O4, can be with repeated recycling utilize with magnetism, but also have production cost low, product purity is high, is suitable for industry
The features such as metaplasia produces., energy consumption not only can be effectively reduced, and can thoroughly solve the problems, such as organic solvent residual, it is green safe
Environmental protection.
Specific embodiment
Below with reference to specific implementation example, the present invention is described in detail；It is a kind of to utilize magnetic mesoporous SiO2@Fe3O4It mentions
Take polysaccharide in Rumex madaio the preparation method comprises the following steps: the step is
(1) fresh Rumex madaio is cleaned, then chooses root, root is placed in 50-70 ° of hothouse and dried to constant
Quality；
(2) dry root is carried out using disintegrating machine being crushed to powder, is placed spare in bottle；
(3) part Rhubarb is weighed, carries out microblogging ultrasonication after ethanol solution is added；After propose heating extraction to after tasteless
Water is added to obtain Radix Et Rhizoma Rhei extract
(4) treated, and Radix Et Rhizoma Rhei extract measures absorbance, and the SiO of equivalent is added after measurement2@Fe3O4Nano particle, finally
To product.
As a preferred embodiment: root being placed in the step (1) in 65 ° of hothouse and dried to constant-quality.
As a preferred embodiment: being added by the mass volume ratio of 1:1 to 1:20 into Rhubarb in the step (3) dense
The ethanol solution for being 20%-95%, and heating and refluxing extraction 1-3 hours are spent, extraction time is 1-3 times, combined extract concentration
It is extremely tasteless, add water to obtain Radix Et Rhizoma Rhei extract,
As a preferred embodiment: the magnetic mesoporous SIO2@Fe3O4The preparation method comprises the following steps: being the electronic balance of a ten thousandth with precision
Precise 2.9-3.0gFeCl respectively3·6H2The FeCl of O and 2.0-3.0g2·4H2O is placed in 250ml three-necked flask, in nitrogen
It is being 140-160g.l by 40-60ml concentration under atmosphere is enclosed-1Aqueous Solutions of Polyethylene Glycol be added in above-mentioned beaker, heating water bath
To 40-60 °, under 900-1100rpm revolving speed, ammonium hydroxide is added, solution pH value adjustment is reacted into 30-40min between 10-12,
With magnet by Fe3O4Nanoparticle is separated with solvent, and Fe is washed with deionized3O4Nanoparticle, the Fe of washing3O4Nanometer
Particle is placed in 250ml flask, by the SiO of 40-60ml concentration2Solution is added to the Fe after washing3O4In flask, then will
Deionized water is added to adjust the PH of mixed solution between 8-9, finally, ultrasonic disperse 10-20min acquisition is magnetic mesoporous
SiO2@Fe3O4Nanoparticle.
SiO2@Fe3O4Nano particle carries out mechanical means to Rumex madaio cell wall using Superparamagnetism mesoporous magnetic field environment
Broken wall.The cavitation bubble of cavitation effect, generation collapsed in very short time at 10 seconds, and the high temperature of 5000K or so can be generated in bubble.
The broken wall rate under the cavitation of ultrasonic wave is accelerated, overflows cell content material more, to have more
Rheum emodin is outflow from cytoplasm, improves extraction efficiency and content.
Claims (4)
1. a kind of utilize magnetic mesoporous SiO2@Fe3O4Extract the preparation method of polysaccharide in Rumex madaio, it is characterised in that the step
For
(1) fresh Rumex madaio is cleaned, then chooses root, root is placed in 50-70 ° of hothouse and dried to constant
Quality；
(2) dry root is carried out using disintegrating machine being crushed to powder, is placed spare in bottle；
(3) part Rhubarb is weighed, carries out microblogging ultrasonication after ethanol solution is added；After propose heating extraction to after tasteless
Water is added to obtain Radix Et Rhizoma Rhei extract
(4) treated, and Radix Et Rhizoma Rhei extract measures absorbance, and the SiO of equivalent is added after measurement2@Fe3O4Nano particle, finally
To product.
2. according to claim 1 utilize magnetic mesoporous SiO2@Fe3O4The preparation method of polysaccharide in Rumex madaio is extracted, it is special
Sign, which is in the step (1) for be placed on root, to be dried in 65 ° of hothouse to constant-quality.
3. according to claim 1 utilize magnetic mesoporous SiO2@Fe3O4The preparation method of polysaccharide in Rumex madaio is extracted, it is special
Sign is that the second that concentration is 20%-95% is added in the step (3) into Rhubarb by the mass volume ratio of 1:1 to 1:20
Alcoholic solution, and heating and refluxing extraction 1-3 hours, extraction time are 1-3 times, and combined extract is concentrated into tasteless, and water is added to obtain rheum officinale
Extracting solution.
4. according to claim 1 utilize magnetic mesoporous SiO2@Fe3O4The preparation method of polysaccharide in Rumex madaio is extracted, it is special
Sign is the magnetic mesoporous SiO2@Fe3O4The preparation method comprises the following steps: distinguishing precise with the electronic balance that precision is a ten thousandth
2.9-3.0gFeCl3.6H2The FeCl of O and 2.0-3.0g2.4H2O is placed in 250ml three-necked flask, under nitrogen atmosphere, is being incited somebody to action
40-60ml concentration is 140-160g.l-1Aqueous Solutions of Polyethylene Glycol be added in above-mentioned beaker, heating water bath to 40-60 °,
Under 900-1100rpm revolving speed, ammonium hydroxide is added, solution pH value adjustment is reacted into 30-40min between 10-12, with magnet by Fe3O4
Nanoparticle is separated with solvent, and Fe is washed with deionized3O4Nanoparticle, the Fe of washing3O4Nanoparticle is placed in
In 250ml flask, by the SiO of 40-60ml concentration2Solution is added to the Fe after washing3O4In flask, then by addition go from
Sub- water adjusts the PH of mixed solution between 8-9, finally, ultrasonic disperse 10-20min obtains magnetic mesoporous SiO2@Fe3O4It receives
Rice corpuscles.
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| CN201811604153.1A CN110078839A (en) | 2018-12-26 | 2018-12-26 | It is a kind of to utilize magnetic mesoporous SiO2@Fe3O4Extract the preparation method of polysaccharide in Rumex madaio |
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| CN201811604153.1A CN110078839A (en) | 2018-12-26 | 2018-12-26 | It is a kind of to utilize magnetic mesoporous SiO2@Fe3O4Extract the preparation method of polysaccharide in Rumex madaio |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114573725A (en) * | 2022-03-02 | 2022-06-03 | 徐州工程学院 | Extraction method of spina date seed polysaccharide extract |
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