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Method for preparing high-purity garlic polysaccharide by co-precipitation of cinchona alkaloid-derived quaternary ammonium salt

A technology of garlic polysaccharide and cinchona alkaloid, applied in the field of phytochemistry, can solve the problems of low effective yield of equipment, not easy to dissociate, and extraction cannot be continuously performed, etc., and achieves the effect of avoiding decomposition of garlic polysaccharide and avoiding quality deviation.

Inactive Publication Date: 2018-12-18
毛雪梅
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, the traditional garlic polysaccharide extraction method often requires a series of complex purification processes such as protein removal, pectin removal, ethanol precipitation, gel column purification, and dialysis to prepare high-purity garlic polysaccharides. The preparation process is extremely cumbersome.
[0004] Compared with traditional garlic polysaccharide extraction methods, some new technologies have emerged in recent years, such as supercritical CO 2 Extraction technology; CN 1818045 A discloses a method using supercritical CO 2 The method of extracting garlic oil and garlic polysaccharide from fresh garlic at the same time, although the process parameters are simple and the process is green and environmentally friendly, but the separation process needs to be carried out under high pressure, the one-time investment in equipment is too large, and the extraction cannot be carried out continuously, resulting in the effective production of the equipment. low rate
It is a simple purification method to use quaternary ammonium salt and acidic polysaccharide to form water-insoluble compound into salt. The commonly used quaternary ammonium salt is cetyltrimethylammonium bromide (CTMAB) and its Methyl ammonium hydroxide (CTA-OH) and cetylpyridinium chloride (CPC), but it is not easy to dissociate after salt formation, resulting in low polysaccharide yield

Method used

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  • Method for preparing high-purity garlic polysaccharide by co-precipitation of cinchona alkaloid-derived quaternary ammonium salt
  • Method for preparing high-purity garlic polysaccharide by co-precipitation of cinchona alkaloid-derived quaternary ammonium salt
  • Method for preparing high-purity garlic polysaccharide by co-precipitation of cinchona alkaloid-derived quaternary ammonium salt

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1) Degreasing pre-treatment: After peeling the garlic, vacuum-dry it at 35-40°C to constant weight, then chop it until the particle size is 200-300 mesh to obtain 5.0kg minced garlic, and put the minced garlic in a 100L stainless steel high-pressure airtight container , add the mixed solution of 25kg acetone and tetrahydrofuran (according to volume ratio calculation, acetone / tetrahydrofuran=95:5), stir and disperse for 10-20min, then add 25kg of dry ice with a particle size of 0.5-1cm from the feed port, close the feed port, and Stir at room temperature, and stop stirring when the temperature in the kettle naturally rises to 0-5°C; press filter to remove the filtrate, and vacuum-dry the filter cake at 35-40°C to constant weight to obtain 4.91kg of degreased primary garlic residue;

[0035] 2) Low-temperature ultrasonic removal of small molecular sugars: Add 4.91kg of defatted primary garlic residues to 27kg of 90% V ethanol aqueous solution, ultrasonicate at 10-20°C for ...

Embodiment 2

[0043] Take 1.0g of Pre-garlic polysaccharide respectively, add 50ml of water to dissolve, then add 50ml of different quaternary ammonium salt solutions with a concentration of 2%wt, let stand at 40°C overnight (8-12h), then cool down to room temperature, centrifuge, After drying, the quality of the precipitate was detected, and the results are shown in Table 1:

[0044] Table 1 Co-precipitation effect of different quaternary ammonium salts on garlic polysaccharides

[0045]

[0046] The above results show that the use of cinchona base quaternary ammonium salt for co-precipitation with garlic polysaccharides can obtain a high-yield precipitate, compared with the traditional cetyltrimethylammonium bromide (CTMAB) and its cetyl Compared with trimethylammonium hydroxide (CTA-OH) and cetylpyridinium chloride (CPC), the yield is greatly improved.

Embodiment 3

[0048] In the present invention, each 1 g of precipitates formed by N-(9-anthracenylmethyl) cinchonaline bromide and N-benzyl cinchonaine bromide is adopted, and 160ml of 2mol / L different inorganic salt aqueous solutions are used at 35-40° C. Carry out dissociation for 4-6 hours, centrifuge to obtain the filtrate, then add absolute ethanol dropwise to the filtrate until no solid precipitates, collect the solid by filtration, dry and weigh it under vacuum at 40-45°C, and obtain high-purity garlic polysaccharide dissociated from different inorganic salts , the weight of garlic polysaccharide obtained by different inorganic salts is shown in Table 2:

[0049] The weight of the garlic polysaccharide obtained by the dissociation of different inorganic salts in table 2

[0050]

[0051] The above results show that different inorganic salts have different dissociation effects, among which ammonium bisulfate has the best dissociation effect; different quaternary ammonium salts have...

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Abstract

The invention belongs to the technical field of phytochemicals, and particularly relates to a method for preparing high-purity garlic polysaccharide by co-precipitation of a cinchona alkaloid-derivedquaternary ammonium salt. The method adopts the cinchona alkaloid-derived quaternary ammonium salt as a precipitating agent to form precipitates with garlic polysaccharide, the precipitates are dissociated in an inorganic salt aqueous solution, the solution is subjected to ultrafiltration so that a dissociating liquid is obtained, and the dissociating liquid is subjected to alcoholysis so that high-purity garlic polysaccharide is obtained. The molecular weight distribution is normal distribution and the average molecular weight is 4380 Da. The method is simple and is easy to control. All processes have key quality control points so that production amplification is promoted.

Description

technical field [0001] The invention belongs to the technical field of phytochemistry, and in particular relates to a method for preparing high-purity garlic polysaccharide by coprecipitation of cinchona quaternary ammonium salt. Background technique [0002] Garlic polysaccharide is the health-care functional ingredient with the highest content in garlic, accounting for 15% to 25% of fresh garlic. It has multiple functions such as proliferating intestinal probiotics, assisting digestion, enhancing immunity, preventing liver damage, anti-oxidation and anti-virus. Garlic polysaccharide has a wide range of practical application prospects in the fields of medicine and food. [0003] At present, the extraction methods of garlic polysaccharides mainly include hot water, dilute salt, dilute alkali and dilute acid extraction, and there are also extraction methods such as compound enzyme treatment and ultrasonic-assisted acceleration of polysaccharide release. Hot water extraction ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/00
CPCC08B37/0003
Inventor 毛雪梅郭腾跃韩康刘景强
Owner 毛雪梅
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