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Rapid preparation method of polygonum multiflorum decolorizing polysaccharide

A technology of polysaccharides from Polygonum multiflorum and Polygonum multiflorum, applied in the field of polysaccharide decolorization of Polygonum multiflorum, can solve the problems of short service life of DEAE cellulose column, large amount of solvent, long decolorization time, etc., to avoid activated carbon or organic solvent residue, simple follow-up processing steps, The effect of high purification and decolorization efficiency

Inactive Publication Date: 2017-02-15
CHONGQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually, the traditional water extraction and alcohol precipitation method is the main method to obtain polysaccharides of Polygonum multiflorum, but the obtained polysaccharides have dark color and many impurities, which seriously affect the purity, color, stability and biological activity of the polysaccharides, and also hinder the research on the polysaccharides. In-depth study on the relationship between polysaccharide structure and its biological activity
[0003] In order to improve the product quality of polysaccharides from Polygonum multiflorum, at present, methods such as activated carbon adsorption, hydrogen peroxide oxidation, DEAE cellulose column chromatography, and macroporous resin adsorption are mainly used for purification and decolorization, but the desired effect cannot be achieved yet.
For example, although the activated carbon adsorption method is economical, the decolorization time is long, the decolorization effect is poor, and the polysaccharide retention rate is low.
Although the decolorization effect of hydrogen peroxide oxidation is good, the reaction process will cause certain damage to the polysaccharide structure and affect its biological activity.
Although DEAE cellulose column chromatography can achieve better decolorization effect, the service life of DEAE cellulose column is short and the cost of use is too high
The macroporous resin adsorption method has defects such as long decolorization time, low decolorization efficiency, small sample processing capacity, and large solvent consumption. For example, in the macroporous resin adsorption method disclosed in patent document CN102731667A, the sample processing concentration is only 5-15g / L, and the decolorization The purification time needs 4-8h, the amount of solvent is huge, and the decolorization efficiency is too low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The preparation of embodiment 1 Polygonum multiflorum polysaccharide crude product

[0044] Step A degreasing: take raw Radix Polygoni Multiflori Radix as raw material, crush Polygonum Polygoni Multiflori without impurities, sieve through a 100-mesh iron sieve, collect the sifted raw material powder with petroleum ether at a volume ratio of 1:8, and place in a water bath environment at 90°C Extract for 0.5h, filter, take the filter residue and repeat petroleum ether degreasing twice; collect the degreased filter residue, evaporate the organic solvent on the surface to obtain the degreasing treated Polygonum multiflorum medicinal material raw material.

[0045] Step B extraction: extract the degreased Polygonum multiflorum raw material obtained in step A and distilled water in a multi-functional extraction tank at 85° C. for 2 hours, and filter , and the filter residue was extracted 3 times. The extracts were collected and combined, and concentrated to 1 / 10 of the origi...

Embodiment 2

[0046] The preparation of embodiment 2 Polygonum multiflorum polysaccharide crude product

[0047] Step A Degreasing: Obtain the defatted Radix Polygoni Multiflori medicinal material raw material with the method of Step A of Example 1.

[0048] Step B extraction: extract the degreased Polygonum multiflorum raw material obtained in step A and distilled water according to the mass (g) volume (mL) solid-liquid ratio of 1:6, extract in a multi-functional extraction tank at 85°C for 2h, filter, and repeat the filter residue Extract 2 times, collect and combine the extracts, and concentrate to 1 / 10 of the original volume.

[0049] Step C Alcohol Precipitation: Cool the Polygonum multiflorum polysaccharide concentrate obtained in Step B to room temperature, add 4 times the volume of absolute ethanol, let it stand at 4°C for 24 hours, centrifuge for 30 minutes at a speed of 3000r / min, take the precipitate and dry it in vacuum to obtain Polygonum multiflorum crude polysaccharides.

...

Embodiment 3

[0051] The preparation of embodiment 3 Polygonum multiflorum decolorization polysaccharide

[0052] The Polygonum multiflorum polysaccharide extract obtained in Example 1 or the Polygonum multiflorum crude polysaccharide obtained in Example 2 and distilled water were dissolved in a mass (g) volume (mL) ratio of 1:20, filtered, and the filtrate was taken as an injection sample.

[0053] Use 400mL of 50-70μm polymethacrylate MCI GEL reverse-phase fine separation filler as the column filler, and use water as the elution solvent. Take 80mL injection sample and pump it into the separation column at a speed of 1.0mL / min. After the injection is completed, absorb for 10min. Adjust the pump flow rate to 10mL / min. The fraction collector collects one tube every 5 minutes, and uses the phenol-sulfuric acid method to detect tube by tube, and collects those with positive reactions. Concentrate and freeze-dry to obtain the decolorized polysaccharide of Polygonum multiflorum, and the product...

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Abstract

The invention belongs to the field of chemistry of traditional Chinese medicines, and relates to a rapid preparation method of polygonum multiflorum decolorizing polysaccharide. The rapid preparation method of the polygonum multiflorum decolorizing polysaccharide, provided by the invention, is simple and convenient to operate, economic, convenient, fast and efficient, and has no influence on a polysaccharide structure and activity; only aqueous phase elution is adopted, no organic solvent is remained, the yield and the purity are high, the content of the polysaccharide achieves 85 percent or more, and the retention rate exceeds 90 percent.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicine chemistry, and relates to a method for preparing polysaccharide decolorization of Polygonum multiflorum with high yield and purity, which is easy to operate, economical, convenient, fast and efficient, has no influence on polysaccharide structure and activity, has no organic solvent residue, and has high yield and purity. Background technique [0002] Polysaccharides of Polygonum multiflorum have biological activities such as anti-aging, immune regulation, anti-oxidation and anti-senile dementia, and are important functional components of Polygonum multiflorum. Usually, the traditional water extraction and alcohol precipitation method is the main method to obtain polysaccharides of Polygonum multiflorum, but the obtained polysaccharides have dark color and many impurities, which seriously affect the purity, color, stability and biological activity of the polysaccharides, and also hinder ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/00
CPCC08B37/0003C08B37/00
Inventor 徐溢张庆牟秀霓曹坤吕君江张晓凤
Owner CHONGQING UNIV
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