CN106432521B - A kind of preparation method of Phosphation bletilla polysaccharide - Google Patents
A kind of preparation method of Phosphation bletilla polysaccharide Download PDFInfo
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- CN106432521B CN106432521B CN201610844043.7A CN201610844043A CN106432521B CN 106432521 B CN106432521 B CN 106432521B CN 201610844043 A CN201610844043 A CN 201610844043A CN 106432521 B CN106432521 B CN 106432521B
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- bletilla polysaccharide
- phosphation
- polysaccharide
- bletilla
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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
Abstract
The present invention provides a kind of preparation methods of Phosphation bletilla polysaccharide, weigh dry bletilla polysaccharide sample, being configured to concentration is 1 ~ 10% solution, sequentially add sodium polyphosphate and sodium sulphate, wherein bletilla polysaccharide, sodium polyphosphate, sodium sulphate mass ratio be (5 ~ 20): (1 ~ 10): 1；PH value of reaction system is adjusted, makes the pH value of reaction system between 4 ~ 6, reaction temperature is 70 ~ 95 DEG C, and the reaction time is 3~6hr, after reaction, through alcohol precipitation, dialysis, dry obtained Phosphation bletilla polysaccharide.The Phosphation bletilla polysaccharide degree of substitution that preparation method of the invention obtains is moderate, solubility property is become reconciled, easy to operate, solves the problems, such as that dissolubility caused by synthesis under alkaline condition is poor.
Description
Technical field
The invention belongs to field of medicinal chemistry, are related to a kind of bletilla polysaccharide, and specifically a kind of Phosphation bletilla striata is more
The preparation method of sugar.
Background technique
The bletilla striata is orchid family bletilla striata category, herbaceos perennial.Alias bletilla, purple blue, purple a species of orchid, hundred large bamboo hats with a conical crown and broad brim etc., there is convergence to stop
Blood, detumescence and promoting granulation, clearing heat and promoting diuresis and other effects use the history of existing nearly one thousand years as medicinal material.Contain in the bulb tissue of the bletilla striata
Water-soluble polysaccharide abundant.
It is higher that the activity of polysaccharide directly or indirectly by its structural constraint, by molecular modification can get bioactivity, uses
The more extensive polysaccharide derivates in way.Polysaccharide molecule method of modifying includes chemistry, biology and physical method.Phosphorylation modification be by
Polysaccharide molecule hydroxyl, carboxyl, amino terminal are replaced with phosphate group, are one of common methods in chemical method.Some natural polysaccharides
Bioactivity significantly improves after phosphorylation modification, for example, can make originally do not have active polysaccharide show it is antitumor,
Antibacterial isoreactivity.
The degree of cross linking of the discovery of existing preparation method, the Phosphation polysaccharide prepared under alkaline condition is high, solubility property compared with
Difference is insoluble in water, alcohol and salting liquid, using limited.
Summary of the invention
For above-mentioned technical problem in the prior art, the present invention provides a kind of preparation sides of Phosphation bletilla polysaccharide
The preparation method of method, this Phosphation bletilla polysaccharide will solve the friendship of the Phosphation polysaccharide prepared in the prior art
Lian Dugao, solubility property is poor, the not high technical problem of bioactivity.
The present invention provides a kind of preparation methods of Phosphation bletilla polysaccharide, include the following steps:
1) bletilla polysaccharide is dissolved in water, is configured to the solution that mass percent concentration is 1~10%；
2) sodium polyphosphate and sodium sulphate are sequentially added into bletilla polysaccharide solution, bletilla polysaccharide, sodium polyphosphate, sodium sulphate
Mass ratio is (5~20): (1~10): 1；
3) pH value of reaction system is adjusted, makes the pH value of reaction system between 4~6, reaction temperature is 70~95 DEG C, reaction
Time is 3~6hr, after reaction, through alcohol precipitation, dialysis, dry obtained Phosphation bletilla polysaccharide.
Further, pH value is adjusted using the hydrochloric acid solution of 0.1~1mol/L.
The present invention changes the soda acid item of product synthesis using Phosphation bletilla polysaccharide dissolubility as important performance assessment criteria
Part optimizes the preparation method of Phosphation bletilla polysaccharide by controlling degree of substitution.The measurement of degree of substitution uses ascorbic acid-molybdenum
Sour ammonium visible spectrophotometer method；Phosphation bletilla polysaccharide Structural Identification uses infrared spectrum spectrogram, and pattern identification uses
SEM figure, crystallization situation use Xrd.Phosphation bletilla polysaccharide antioxygenic property prepared by the method for the present invention is strong, low dense
Degree is lower to have higher Hydroxyl radical-scavenging ability.
The present invention is compared with prior art, and technological progress is significant.It is moderate, molten that the present invention provides a kind of degree of substitution
It is good to solve performance, easy to operate, the preparation method for the Phosphation bletilla polysaccharide that reaction reagent easily obtains, phosphate prepared by the present invention
Change the control of bletilla polysaccharide degree of substitution between 0.030~0.052, it is soluble easily in water.It is more that the present invention prepares the bletilla striata in acid condition
The method of sugar phosphate, easy to operate, reaction condition is mild, solves asking for dissolubility difference caused by synthesis under alkaline condition
Topic, product have good dissolubility energy and antioxygenic property.
Detailed description of the invention
Fig. 1 is the infrared spectrogram for the Phosphation bletilla polysaccharide that embodiment 1 obtains.
Fig. 2 is the morphology characterization for the Phosphation bletilla polysaccharide that embodiment 1 obtains.
Fig. 3 is the electron-microscope scanning figure for the Phosphation bletilla polysaccharide that embodiment 1 obtains.
Fig. 4 is the Phosphation bletilla polysaccharide X single crystal diffraction curve that embodiment 1 obtains.
Fig. 5 is Phosphation bletilla polysaccharide dissolution time and temperature relation figure.
Fig. 6 is Phosphation bletilla polysaccharide Scavenging action to hydroxyl free radical figure.
Specific embodiment
The present invention is made with specific embodiment with reference to the accompanying drawings of the specification and further being elaborated, the embodiment
It is served only for explaining the present invention, be not intended to limit the scope of the present invention.Experimental method used in following embodiments is such as without spy
Different explanation, is conventional method；Used material, reagent etc., unless otherwise specified, for the reagent commercially obtained
And material.
The present invention changes the soda acid item of product synthesis using Phosphation bletilla polysaccharide dissolubility as important performance assessment criteria
Part optimizes the preparation method of Phosphation bletilla polysaccharide by controlling degree of substitution.The measurement choosing of Phosphation bletilla polysaccharide degree of substitution
With ascorbic acid-ammonium molybdate visible spectrophotometer method.
Embodiment 1
It weighs 1g bletilla polysaccharide to be dissolved in 20mL distilled water, stirring is complete to dissolving.Heat temperature raising reaches 90 DEG C to temperature
Successively by the polyphosphoric acids sodium solution of 10ml 0.05g/ml, the metabisulfite solution of 25ml 5g/L is added reaction vessel, uses 1mol/
The HCl of L adjusts pH=4, and stirring in water bath reacts 4hr, and 3 times of volume dehydrated alcohols are then added, and alcohol precipitation is overnight, and decompression filters, will
The a small amount of water of product, which dissolves, is placed in bag filter distilled water dialysis r for 24 hours, is freeze-dried to obtain bletilla polysaccharide phosphate, degree of substitution
It is 0.036.
Embodiment 2
It weighs 1g bletilla polysaccharide to be dissolved in 20mL distilled water, stirring is complete to dissolving.Heat temperature raising reaches 80 DEG C to temperature
Successively by the polyphosphoric acids sodium solution of 20ml 0.05g/ml, the metabisulfite solution of 25ml 5g/L is added reaction vessel, uses 1mol/
The HCl of L adjusts pH=5, and stirring in water bath reacts 5hr, and 3 times of volume dehydrated alcohols are then added, and alcohol precipitation is overnight, and decompression filters, will
The a small amount of water of product, which dissolves, is placed in bag filter distilled water dialysis r for 24 hours, is freeze-dried to obtain bletilla polysaccharide phosphate, degree of substitution
It is 0.042.
Embodiment 3
It weighs 1g bletilla polysaccharide to be dissolved in 20mL distilled water, stirring is complete to dissolving.Heat temperature raising reaches 90 DEG C to temperature
Successively by the polyphosphoric acids sodium solution of 15ml 0.05g/ml, the metabisulfite solution of 25ml 5g/L is added reaction vessel, uses 1mol/
The HCl of L adjusts pH=6, and stirring in water bath reacts 6hr, and 3 times of volume dehydrated alcohols are then added, and alcohol precipitation is overnight, and decompression filters, will
The a small amount of water of product, which dissolves, is placed in bag filter distilled water dialysis r for 24 hours, is freeze-dried to obtain bletilla polysaccharide phosphate, degree of substitution
It is 0.041.
Embodiment 4
It weighs 1g bletilla polysaccharide to be dissolved in 20mL distilled water, stirring is complete to dissolving.Heat temperature raising reaches 95 DEG C to temperature
Successively by the polyphosphoric acids sodium solution of 10ml 0.05g/ml, the metabisulfite solution of 25ml 5g/L is added reaction vessel, uses 1mol/
The HCl of L adjusts pH=5, and stirring in water bath reacts 3hr, and 3 times of volume dehydrated alcohols are then added, and alcohol precipitation is overnight, and decompression filters, will
The a small amount of water of product, which dissolves, is placed in bag filter distilled water dialysis r for 24 hours, is freeze-dried to obtain bletilla polysaccharide phosphate, degree of substitution
It is 0.032.
5 Phosphation bletilla polysaccharide solvability of embodiment:
50mL distilled water is added in 1g Phosphation bletilla polysaccharide, 10min is infiltrated at room temperature, beaker is put into not equality of temperature
In the water bath of degree, it is completely dissolved using blender (0.15Kr/min) stirring to polysaccharide.
As shown in Figure 5, Phosphation bletilla polysaccharide substantially can all dissolve within 30 minutes.
6 Phosphation bletilla polysaccharide Hydroxyl radical-scavenging ability of embodiment:
By 1.5mL FeSO4(1.5mmol/L), 0.5mL H2O2(6mmol/L), 0.5mL sodium salicylate (20mmol/L) point
It is not added in the polysaccharide phosphate ester solution of 1mL various concentration；37 DEG C of water-bath culture 1h survey salicylate mixture in 562nm
Absorbance A s；1ml water replaces polysaccharide phosphate ester solution to obtain A0；0.5ml water replaces sodium salicylate solution to obtain Ac；Each sample
Product work is parallel three times, takes its average value.Clearance rate calculates as follows:
Clearance rate (%)=[A0- (AS-AC)]/A0 × 100%
According to above-mentioned formula, clearance rate more high anti-oxidation effect is better.
It will be appreciated from fig. 6 that the Hydroxyl radical-scavenging ability of Phosphation bletilla polysaccharide is up to 85% or more.
Although the embodiment of the present invention is described above, it is to be understood that above-described embodiment is exemplary, no
It can be interpreted as limitation of the invention, those skilled in the art can carry out above-described embodiment within the scope of the invention
Variation, modification, replacement, modification.
Claims (2)
1. a kind of preparation method of Phosphation bletilla polysaccharide, it is characterised in that include the following steps:
1) bletilla polysaccharide is dissolved in water, is configured to the solution that mass percent concentration is 1-10%；
2) sodium polyphosphate and sodium sulphate are sequentially added into bletilla polysaccharide solution, bletilla polysaccharide, sodium polyphosphate, sodium sulfate quality
Than being 8:(4-8): 1；
3) pH value of reaction system is adjusted, makes the pH value of reaction system between 4-6, reaction temperature is 80-95 DEG C, and the reaction time is
3-6hr, after reaction, through alcohol precipitation, dialysis, dry obtained Phosphation bletilla polysaccharide.
2. a kind of preparation method of Phosphation bletilla polysaccharide according to claim 1, it is characterised in that: use 0.1-
The hydrochloric acid solution of 1mol/L adjusts pH value.
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| CN109265572A (en) * | 2018-09-21 | 2019-01-25 | 湖南大学 | A kind of phosphorylation polyhydroxy high-molecular compound and its synthetic method |
| CN112480280B (en) * | 2020-12-08 | 2022-06-24 | 中国科学院新疆理化技术研究所 | Preparation method and application of bletilla striata polysaccharide derivative |
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