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Modified macroporous polyvinyl alcohol resin and method for separating and purifying Chinese medicinal herb polysaccharide

A polyvinyl alcohol and resin separation technology, applied in chemical instruments and methods, ion exchange, and other chemical processes, can solve problems such as time-consuming, high resource and energy consumption, pollution, etc., and achieve simple process, resource and energy low cost effect

Inactive Publication Date: 2010-09-08
TIANJIN DEOUTE BIOLOGY MEDICINE SICENCE & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Most of the above extraction and separation methods need complex steps such as water extraction, alcohol precipitation, deproteinization, decolorization, desalination, etc., and all need to use a large amount of organic solvents such as petroleum ether, chloroform, ethanol, acetone, etc. The whole process is time-consuming. Long, resource and energy consumption is large, and will produce pollution, the environment is not friendly
These greatly limit the production and application of Chinese herbal polysaccharides

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1. Preparation of modified macroporous polyvinyl alcohol separation resin

[0029] 40g of polyvinyl alcohol microspheres with an average particle size of 60 mesh (copolymer of vinyl acetate and triallyl isocyanurate; degree of crosslinking is 30%, degree of alcoholysis 90%, produced by Tianjin Ou Rui Biotechnology Co., Ltd.), adding 80ml of 2M NaOH solution, 160ml of epichlorohydrin and 100ml of DMSO (dimethyl sulfoxide), shaken and reacted at 40°C for 3h, washed thoroughly with distilled water, and dried to obtain activated microspheres with an epoxy value of 120μmol / g (determined by magnesium chloride-hydrochloric acid titration). Add 200ml of 2M NaOH solution and 200ml of trimethylamine to the activated PVA resin, shake and react at 40°C for 10h, and then fully wash with distilled water. That is, polyvinyl alcohol separation microsphere resin was obtained, and the exchange capacity of the microspheres was 100 μmol / g (determined by acid-base titration met...

Embodiment 2

[0030] Example 2. Separation and purification of crude licorice polysaccharide by modified macroporous polyvinyl alcohol separation resin

[0031] Get 20ml of the resin prepared by Example 1 and pack it into a separation column, the diameter of the separation column is 15mm, and the height of the resin is 150mm. Get crude licorice polysaccharide thick (purity 10.26%, protein content 6.58mg) and be made into the solution of 4mg / ml concentration with distilled water, filter and remove a small amount of insoluble precipitation to obtain crude licorice polysaccharide clear liquid, this clear liquid is 1BV / h (BV: bed volume ) through the separation column, receive the effluent, and detect the polysaccharides, proteins and pigments in the effluent and sample solution respectively. The effluent was freeze-dried to obtain 9.8 mg of white polysaccharide powder, with a purity of 87.59% (measured by phenol-sulfuric acid colorimetry), a yield of 8.17%, and a one-time protein removal rate ...

Embodiment 3

[0032] Example 3. Separation and purification of crude Ganoderma lucidum polysaccharide by modified macroporous polyvinyl alcohol separation resin

[0033]Get the resin prepared by embodiment 1 and pack the separation column by the method of embodiment 2. Get crude Ganoderma lucidum polysaccharide (purity 15.4%, protein content 0.474mg) and be made into the solution of 4mg / ml concentration with distilled water, filter and remove a small amount of insoluble precipitation to obtain crude licorice polysaccharide supernatant, this supernatant passes through the separation column with the flow velocity of 1BV / h, Receive the effluent and detect the polysaccharides, proteins and pigments in the effluent and sample solution respectively. The separated liquid was freeze-dried to obtain 10.5 mg of white polysaccharide powder with a purity of 91.39%, a yield of 8.75%, a one-time protein removal rate of 88.23%, and a pigment removal rate of 92.41%. (The detection method is the same as ab...

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PUM

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Abstract

The present invention relates to a modified macroporous polyvinyl alcohol separation resin and the method of separating and purifying herbal medical polysaccharide. The polyvinyl alcohol resin microsphere is reacted with epichlorohydrin under an alkaline condition and then is reacted with trimethylamine, triethylamine or diethylenetriamine under the alkaline condition and washed by water and dried. An aqueous solution of crude polysaccharide (such as a glycyrrhizae polysaccharide, a milk vetch root polysaccharide, a ganoderma polysaccharide, a mushroom polysaccharide, a ginseng polysaccharideetc) is directly separated and purified by the modified macroporous polyvinyl alcohol separation resin column, and 85 percent of the major impurity of protein and pigment in the aqueous solution of crude polysaccharide can be removed only by one step, and the separation liquid can be dried to obtain a polysaccharide product, the purity of which is more than 80 percent.

Description

technical field [0001] The invention relates to the field of preparation of separation resin and extraction of effective components of Chinese herbal medicine, in particular to a modified macroporous polyvinyl alcohol resin and a method for separating and purifying polysaccharides of Chinese herbal medicine. The resin involved in the invention can simply and effectively remove proteins, pigments and the like in crude polysaccharides in Chinese herbal medicines, thereby achieving the purpose of separating and purifying the crude polysaccharides. Background technique [0002] Polysaccharides, also known as polysaccharides, generally have a molecular weight of tens of thousands to millions, and are widely found in animal cell membranes, plant and microbial cell walls, and are polymers linked by aldose or ketose through glycosidic bonds. . So far, more than 300 kinds of polysaccharides have been extracted from natural products, among which the water-soluble polysaccharides obta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/08B01J20/26
Inventor 欧来良孔德领俞耀庭王为超张华杨佳玲向才虎
Owner TIANJIN DEOUTE BIOLOGY MEDICINE SICENCE & TECH
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