CN110372892B - Preparation method of peach gum polysaccharide nanospheres - Google Patents
Preparation method of peach gum polysaccharide nanospheres Download PDFInfo
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- CN110372892B CN110372892B CN201910751060.XA CN201910751060A CN110372892B CN 110372892 B CN110372892 B CN 110372892B CN 201910751060 A CN201910751060 A CN 201910751060A CN 110372892 B CN110372892 B CN 110372892B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/07—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from polymer solutions
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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Abstract
The invention discloses a preparation method of peach gum polysaccharide nanospheres. Adding 1 part by weight of water-soluble peach gum polysaccharide, 4-8 parts by weight of lipoic acid and 0.2-0.8 part by weight of p-toluenesulfonic acid into 50-100 parts by weight of dimethyl sulfoxide, stirring the obtained mixed solution at 80-120 ℃ for 5-12 hours in a nitrogen atmosphere, dialyzing for 24 hours with deionized water, performing centrifugal separation, and collecting precipitate obtained by centrifugation; and adding the collected centrifugal precipitate into 10-50 parts by weight of organic solvent, stirring for 10 minutes, and dialyzing in deionized water for 24 hours to obtain the peach gum polysaccharide nanospheres. The peach gum polysaccharide nanospheres prepared by the method have narrow size distribution, good water dispersibility and stability, simple preparation process, rich raw material sources and low preparation cost. The peach gum polysaccharide nanosphere has good application prospect in the fields of food, cosmetics, biological medicine and the like.
Description
Technical Field
The invention belongs to the field of natural high polymer materials, and particularly relates to a preparation method of peach gum polysaccharide nanospheres.
Background
The natural polymer nanosphere has good application prospect in the fields of drug delivery, environmental management, food, cosmetics and the like due to excellent biocompatibility and rich surface groups. The peach gum polysaccharide is a typical natural polysaccharide, has the characteristics similar to other polysaccharides, namely has good biocompatibility, biodegradability, abundant reactive groups and the like, and is suitable for preparing nanospheres capable of loading functional substances (such as drug molecules, food additives, fluorescent molecules and the like). The peach gum polysaccharide resource in China is very rich, but only a few peach gum polysaccharides are utilized, and the waste of the peach gum polysaccharide resource is very serious. So far, no report has been made on the work of preparing nanospheres from the peach gum polysaccharide. Therefore, the preparation method of the peach gum polysaccharide nanosphere greatly improves the practicability and the added value of the peach gum polysaccharide and powerfully promotes the development and the application of peach gum resources.
Disclosure of Invention
The invention aims to provide a preparation method of peach gum polysaccharide nanospheres, which is characterized in that lipoic acid molecules are utilized to covalently modify peach gum polysaccharide molecules to obtain amphiphilic peach gum polysaccharide molecules, and then the amphiphilic peach gum polysaccharide molecules are self-assembled and crosslinked in water to prepare the peach gum polysaccharide nanospheres.
The method comprises the following specific steps:
(1) adding 1 weight part of water-soluble peach gum polysaccharide, 4-8 weight parts of lipoic acid and 0.2-0.8 weight part of p-toluenesulfonic acid into 50-100 weight parts of dimethyl sulfoxide, stirring and reacting the obtained mixed solution at 80-120 ℃ for 5-12 hours under the nitrogen atmosphere, dialyzing for 24 hours by using deionized water, performing centrifugal separation, and collecting precipitate obtained by centrifugation.
(2) And (2) adding the centrifugal precipitate collected in the step (1) into 10-50 parts by weight of organic solvent, stirring for 10 minutes, and dialyzing in deionized water for 24 hours to obtain the peach gum polysaccharide nanospheres.
The organic solvent is one of ethanol, isopropanol, diethylene glycol, tetrahydrofuran, dimethyl sulfoxide and dimethylformamide.
The chemical reagents are all chemically pure or above.
The invention has the advantages of easily obtained raw materials, simple preparation process, low preparation cost and the like; the prepared peach gum polysaccharide nanospheres have excellent water dispersibility and stability, and the water dispersion liquid can stand for one month without obvious precipitate; the shape and size of the material are tested by a scanning electron microscope and a transmission electron microscope, and the result proves that the material has a spherical structure, the size distribution is narrow, and the size is 20-120 nanometers; in addition, the peach gum polysaccharide nanosphere has good application prospects in the aspects of food, cosmetics, biological medicines and the like.
Drawings
Fig. 1 is a photograph of an aqueous dispersion of the peach gum polysaccharide nanospheres prepared in example 1 of the present invention.
Fig. 2 is a scanning electron microscope photograph of the peach gum polysaccharide nanospheres prepared in example 1 of the present invention.
Fig. 3 is a transmission electron microscope photograph of the peach gum polysaccharide nanospheres prepared in example 1 of the present invention.
Detailed Description
Example 1:
(1) adding 1 g of water-soluble peach gum polysaccharide, 7 g of lipoic acid and 0.2 g of p-toluenesulfonic acid into 50 g of dimethyl sulfoxide, stirring and reacting the obtained mixed solution for 8 hours at 100 ℃ in a nitrogen atmosphere, dialyzing the reacted mixed solution for 24 hours by using deionized water, performing centrifugal separation, and collecting the precipitate obtained by centrifugation.
(2) And (2) adding the centrifugal precipitate collected in the step (1) into 20 g of ethanol, stirring for 10 minutes, and dialyzing in deionized water for 24 hours to obtain the peach gum polysaccharide nanospheres.
Example 2:
(1) adding 1.5 g of water-soluble peach gum polysaccharide, 6 g of lipoic acid and 0.6 g of p-toluenesulfonic acid into 100 g of dimethyl sulfoxide, stirring and reacting the obtained mixed solution at 80 ℃ for 12 hours under the atmosphere of nitrogen, dialyzing the reacted mixed solution with deionized water for 24 hours, performing centrifugal separation, and collecting the precipitate obtained by centrifugation.
(2) And (2) adding the centrifugal precipitate collected in the step (1) into 50 g of ethanol, stirring for 10 minutes, and dialyzing in deionized water for 24 hours to obtain the peach gum polysaccharide nanospheres.
Example 3:
(1) adding 2 g of water-soluble peach gum polysaccharide, 16 g of lipoic acid and 0.8 g of p-toluenesulfonic acid into 100 g of dimethyl sulfoxide, stirring and reacting the obtained mixed solution for 5 hours at 110 ℃ in the nitrogen atmosphere, dialyzing the reacted mixed solution for 24 hours by using deionized water, performing centrifugal separation, and collecting the precipitate obtained by centrifugation.
(2) Adding the centrifugal precipitate collected in the step (1) into 20 g of isopropanol, stirring for 10 minutes, and dialyzing in deionized water for 24 hours to obtain the peach gum polysaccharide nanospheres.
Example 4:
(1) adding 1.8 g of water-soluble peach gum polysaccharide, 10 g of lipoic acid and 1 g of p-toluenesulfonic acid into 125 g of dimethyl sulfoxide, stirring and reacting the obtained mixed solution for 6 hours at 120 ℃ in a nitrogen atmosphere, dialyzing the reacted mixed solution for 24 hours by using deionized water, performing centrifugal separation, and collecting the precipitate obtained by centrifugation.
(2) Adding the centrifugal precipitate collected in the step (1) into 90 g of isopropanol, stirring for 10 minutes, and dialyzing in deionized water for 24 hours to obtain the peach gum polysaccharide nanospheres.
Example 5:
(1) adding 1 g of water-soluble peach gum polysaccharide, 6 g of lipoic acid and 0.8 g of p-toluenesulfonic acid into 100 g of dimethyl sulfoxide, stirring and reacting the obtained mixed solution for 10 hours at 90 ℃ in the nitrogen atmosphere, dialyzing the reacted mixed solution for 24 hours by using deionized water, performing centrifugal separation, and collecting the precipitate obtained by centrifugation.
(2) Adding the centrifugal precipitate collected in the step (1) into 25 g of diglycol, stirring for 10 minutes, and dialyzing in deionized water for 24 hours to obtain the peach gum polysaccharide nanospheres.
Example 6:
(1) adding 2 g of water-soluble peach gum polysaccharide, 10 g of lipoic acid and 1 g of p-toluenesulfonic acid into 120 g of dimethyl sulfoxide, stirring the obtained mixed solution at 85 ℃ in a nitrogen atmosphere for reacting for 9 hours, dialyzing the reacted mixed solution with deionized water for 24 hours, performing centrifugal separation, and collecting the precipitate obtained by centrifugation.
(2) Adding the centrifugal precipitate collected in the step (1) into 60 g of tetrahydrofuran, stirring for 10 minutes, and dialyzing in deionized water for 24 hours to obtain the peach gum polysaccharide nanospheres.
Example 7:
(1) adding 1 g of water-soluble peach gum polysaccharide, 7 g of lipoic acid and 0.6 g of p-toluenesulfonic acid into 70 g of dimethyl sulfoxide, stirring and reacting the obtained mixed solution for 8 hours at 95 ℃ in a nitrogen atmosphere, dialyzing the reacted mixed solution for 24 hours by using deionized water, performing centrifugal separation, and collecting the precipitate obtained by centrifugation.
(2) Adding the centrifugal precipitate collected in the step (1) into 40 g of dimethyl sulfoxide, stirring for 10 minutes, and dialyzing in deionized water for 24 hours to obtain the peach gum polysaccharide nanospheres.
Example 8:
(1) adding 2 g of water-soluble peach gum polysaccharide, 13 g of lipoic acid and 1 g of p-toluenesulfonic acid into 150 g of dimethyl sulfoxide, stirring and reacting the obtained mixed solution at 90 ℃ for 10 hours under the nitrogen atmosphere, dialyzing the reacted mixed solution for 24 hours by using deionized water, performing centrifugal separation, and collecting the precipitate obtained by centrifugation.
(2) And (2) adding the centrifugal precipitate collected in the step (1) into 40 g of dimethylformamide, stirring for 10 minutes, and dialyzing in deionized water for 24 hours to obtain the peach gum polysaccharide nanospheres.
Claims (1)
1. A preparation method of peach gum polysaccharide nanospheres is characterized by comprising the following specific steps:
(1) adding 1 part by weight of water-soluble peach gum polysaccharide, 4-8 parts by weight of lipoic acid and 0.2-0.8 part by weight of p-toluenesulfonic acid into 50-100 parts by weight of dimethyl sulfoxide, stirring and reacting the obtained mixed solution at 80-120 ℃ for 5-12 hours in a nitrogen atmosphere, dialyzing with deionized water for 24 hours, performing centrifugal separation, and collecting precipitate obtained by centrifugation;
(2) adding the centrifugal precipitate collected in the step (1) into 10-50 parts by weight of organic solvent, stirring for 10 minutes, and dialyzing in deionized water for 24 hours to obtain peach gum polysaccharide nanospheres;
the organic solvent is one of ethanol, isopropanol, diethylene glycol, tetrahydrofuran, dimethyl sulfoxide and dimethylformamide;
the chemical reagents are all chemically pure or above.
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Application publication date: 20191025 Assignee: Changsha Houcheng Nanomaterial Technology Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2022450000493 Denomination of invention: A Preparation Method of Peach Gum Polysaccharide Nanospheres Granted publication date: 20220325 License type: Common License Record date: 20221229 |