CN117402266A - Peach gum polysaccharide with high oxidation resistance and preparation method thereof - Google Patents
Peach gum polysaccharide with high oxidation resistance and preparation method thereof Download PDFInfo
- Publication number
- CN117402266A CN117402266A CN202311380715.XA CN202311380715A CN117402266A CN 117402266 A CN117402266 A CN 117402266A CN 202311380715 A CN202311380715 A CN 202311380715A CN 117402266 A CN117402266 A CN 117402266A
- Authority
- CN
- China
- Prior art keywords
- peach gum
- polysaccharide
- gum polysaccharide
- crude
- resistance
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 235000006040 Prunus persica var persica Nutrition 0.000 title claims abstract description 189
- 150000004676 glycans Chemical class 0.000 title claims abstract description 122
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 122
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 122
- 230000003647 oxidation Effects 0.000 title claims abstract description 25
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 240000005809 Prunus persica Species 0.000 title description 2
- 244000144730 Amygdalus persica Species 0.000 claims abstract description 187
- 230000007062 hydrolysis Effects 0.000 claims abstract description 45
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 230000008961 swelling Effects 0.000 claims abstract description 38
- 239000000843 powder Substances 0.000 claims abstract description 34
- 239000000725 suspension Substances 0.000 claims abstract description 31
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003513 alkali Substances 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 17
- 238000004108 freeze drying Methods 0.000 claims abstract description 13
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 9
- 239000002537 cosmetic Substances 0.000 claims abstract description 6
- 235000013376 functional food Nutrition 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 20
- 150000007530 organic bases Chemical class 0.000 claims description 17
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 8
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 150000003141 primary amines Chemical class 0.000 claims description 7
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 5
- 239000003519 biomedical and dental material Substances 0.000 claims description 2
- 230000003078 antioxidant effect Effects 0.000 claims 5
- 238000000502 dialysis Methods 0.000 abstract description 22
- 239000000463 material Substances 0.000 abstract description 7
- 238000011161 development Methods 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 19
- 229910021641 deionized water Inorganic materials 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 17
- 239000007864 aqueous solution Substances 0.000 description 16
- 238000007710 freezing Methods 0.000 description 10
- 230000008014 freezing Effects 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000003301 hydrolyzing effect Effects 0.000 description 9
- 230000002000 scavenging effect Effects 0.000 description 9
- 229960001124 trientine Drugs 0.000 description 7
- OHDRQQURAXLVGJ-HLVWOLMTSA-N azane;(2e)-3-ethyl-2-[(e)-(3-ethyl-6-sulfo-1,3-benzothiazol-2-ylidene)hydrazinylidene]-1,3-benzothiazole-6-sulfonic acid Chemical compound [NH4+].[NH4+].S/1C2=CC(S([O-])(=O)=O)=CC=C2N(CC)C\1=N/N=C1/SC2=CC(S([O-])(=O)=O)=CC=C2N1CC OHDRQQURAXLVGJ-HLVWOLMTSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000002035 prolonged effect Effects 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 230000002292 Radical scavenging effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000007529 inorganic bases Chemical class 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- -1 ABTS radical Chemical class 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- QKUSRAKPUWQSJS-UHFFFAOYSA-N diazanium 3-ethyl-2H-1,3-benzothiazole-6-sulfonate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)C1=CC=C2N(CC)CSC2=C1.[O-]S(=O)(=O)C1=CC=C2N(CC)CSC2=C1 QKUSRAKPUWQSJS-UHFFFAOYSA-N 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- ZHNUHDYFZUAESO-UHFFFAOYSA-N formamide Substances NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000013538 functional additive Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/125—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives containing carbohydrate syrups; containing sugars; containing sugar alcohols; containing starch hydrolysates
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/715—Polysaccharides, i.e. having more than five saccharide radicals attached to each other by glycosidic linkages; Derivatives thereof, e.g. ethers, esters
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
- A61K36/736—Prunus, e.g. plum, cherry, peach, apricot or almond
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
- A61P17/18—Antioxidants, e.g. antiradicals
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P39/00—General protective or antinoxious agents
- A61P39/06—Free radical scavengers or antioxidants
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
-
- 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
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/52—Stabilizers
- A61K2800/522—Antioxidants; Radical scavengers
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Animal Behavior & Ethology (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Engineering & Computer Science (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Molecular Biology (AREA)
- Biochemistry (AREA)
- Epidemiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Dermatology (AREA)
- General Chemical & Material Sciences (AREA)
- Mycology (AREA)
- Toxicology (AREA)
- Nutrition Science (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Microbiology (AREA)
- Alternative & Traditional Medicine (AREA)
- Food Science & Technology (AREA)
- Sustainable Development (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Materials Engineering (AREA)
- Birds (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention provides high-antioxidant peach gum polysaccharide and a preparation method thereof, and belongs to the technical field of natural polysaccharide. According to the invention, organic alkali is used for carrying out nitrogen doping on peach gum polysaccharide, crude peach gum is crushed into crude peach gum powder, then water and organic alkali are added for swelling to obtain crude peach gum suspension, and the crude peach gum suspension is subjected to oil bath hydrolysis, dialysis and freeze drying to obtain the high-oxidation-resistance peach gum polysaccharide. The preparation method provided by the invention has the advantages of simple preparation process, low cost and the like, solves the problem of poor oxidation resistance of the peach gum polysaccharide, and has good application prospect in the fields of cosmetics, functional foods and biomedical materials, and is expected to promote the application of the peach gum polysaccharide and the development and utilization of natural peach gum resources.
Description
Technical Field
The invention belongs to the technical field of natural polysaccharides, and particularly relates to a peach gum polysaccharide with high oxidation resistance and a preparation method thereof.
Background
Natural polysaccharide is a natural polymer with rich sources and good biocompatibility, and is widely applied in various fields. Oxidation resistance is an important factor affecting the application of natural polysaccharide, and natural polysaccharide with good oxidation resistance can play an important role in preventing and treating diseases. In contrast, natural polysaccharides with poor oxidation resistance are limited in application.
The peach gum polysaccharide is a natural polysaccharide extracted from natural crude peach gum. Although the natural peach gum is very abundant in yield, the utilization rate of the natural peach gum is low, because the peach gum polysaccharide prepared by the traditional hydrolysis method has poor oxidation resistance to a certain extent, so that the application of the natural peach gum polysaccharide is limited. In order to overcome the problem, the conventional method is to chemically modify the prepared peach gum polysaccharide, but the conventional modification method has the defects of complex operation process, long reaction period, certain pollution to the environment, high preparation cost and the like, and is difficult to realize large-scale preparation and application. In order to avoid the problem of high cost caused by complicated preparation process and greatly improve the practicability of preparing the peach gum polysaccharide, the invention of a simple and effective method for preparing the peach gum polysaccharide with high oxidation resistance is urgently needed in the field.
Disclosure of Invention
The water-soluble peach gum polysaccharide prepared by the traditional hydrolysis method of the natural crude peach gum has poor oxidation resistance, and severely limits the application of the natural crude peach gum polysaccharide serving as a carrier material or a functional additive in the aspects of cosmetics, functional foods, biomedical materials and the like. In order to solve the technical problems, the invention provides the high-oxidation-resistance peach gum polysaccharide and the preparation method thereof, and the method can realize nitrogen doping during hydrolysis of natural crude peach gum which is insoluble in water, so that the peach gum polysaccharide with excellent water solubility and oxidation resistance is obtained, and the nitrogen-doped high-oxidation-resistance peach gum polysaccharide has good application prospects in the fields of cosmetics, functional foods and biomedical materials.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the invention provides a preparation method of high-oxidation-resistance peach gum polysaccharide, which uses organic alkali to carry out nitrogen doping on the peach gum polysaccharide to obtain the high-oxidation-resistance peach gum polysaccharide.
Further, the organic base is an organic amine containing a primary amine. The organic base selected by the invention is an organic compound containing amino in the molecule, and the organic base is an organic amine containing primary amine, so that the nitrogen atom on the primary amine has strong nucleophilicity and can react with peach gum polysaccharide more easily to realize nitrogen doping.
Still further, the organic base includes one or more of ethylenediamine, diethylenetriamine and triethylenetetramine.
Further, the method comprises the following steps:
crushing the crude peach gum into crude peach gum powder, adding water and organic alkali for swelling to obtain crude peach gum suspension, carrying out oil bath hydrolysis on the crude peach gum suspension, dialyzing and freeze-drying to obtain the high-oxidation-resistance peach gum polysaccharide.
Further, the particle size of the crude peach gum powder is 30-50 meshes.
Further, the volume ratio of the crude peach gum powder to the water to the organic alkali is 1:15-20:0.1-1.
Further, the swelling temperature is 20 to 35 ℃ (room temperature), and the swelling time is 4 to 8 hours.
Further, the swelling specifically comprises the following steps: crushing the crude peach gum into peach gum powder by a crusher, adding deionized water and organic alkali at 20-35 ℃ for full swelling, and stirring the mixture by a stirrer after swelling to obtain the peach gum suspension.
Further, the temperature of the oil bath hydrolysis is 90-110 ℃, the hydrolysis time of the oil bath hydrolysis is 2-8 hours, and the stirring speed is 1000-2000 rpm.
Further, placing the peach gum suspension in an oil bath, stirring, heating and hydrolyzing, placing the peach gum suspension in a dialysis bag for dialysis after the hydrolysis is finished, freezing the peach gum suspension in a refrigerator (-4 to minus 24 ℃), and then freeze-drying the peach gum suspension.
The invention also provides the peach gum polysaccharide with high oxidation resistance, which is prepared by the preparation method.
The invention also provides application of the high-antioxidant peach gum polysaccharide in the fields of cosmetics, functional foods and biomedical material preparation.
Compared with the prior art, the invention has the following advantages and technical effects:
(1) The invention uses nitrogen doping technology to improve oxidation resistance of natural polysaccharide for the first time, and the conventional nitrogen doping technology is based on post-functionalization modification, has the defects of complex operation process and high cost, and is different from the conventional nitrogen doping technology in that the invention uses organic alkali to hydrolyze natural crude peach gum under alkaline conditions, and simultaneously carboxyl contained in peach gum polysaccharide can react with amino contained in organic alkali to realize hydrolysis of natural peach gum and nitrogen doping of peach gum polysaccharide. In addition, the prepared nitrogen-doped peach gum polysaccharide has excellent water solubility and oxidation resistance due to the doping of nitrogen element.
(2) The preparation method provided by the invention has the advantages of simple preparation process, short preparation period, low cost, capability of preparing a large amount and the like, solves the problem of poor oxidation resistance of the peach gum polysaccharide, and has good application prospect in the fields of cosmetics, functional foods and biomedical materials, and is hopeful to promote the application of the peach gum polysaccharide and the development and utilization of natural peach gum resources.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application, illustrate and explain the application and are not to be construed as limiting the application. In the drawings:
FIG. 1 is a photograph of nitrogen-doped high oxidation resistance peach gum polysaccharide prepared in example 1 of the present invention;
FIG. 2 is a photograph of the nitrogen-doped high oxidation resistance peach gum polysaccharide prepared in example 1 of the present invention after dissolution with water;
FIG. 3 is a full spectrum of X-ray photoelectron spectroscopy of the nitrogen-doped high oxidation resistance peach gum polysaccharide prepared in example 1 of the present invention;
FIG. 4 is a graph of N1s spectrum of nitrogen-doped high oxidation resistance peach gum polysaccharide prepared in example 1 of the present invention;
FIG. 5 shows the results of the determination of the ABTS radical clearance of peach gum polysaccharide from example 1 (nitrogen-doped peach gum polysaccharide) and comparative example 1 (undoped peach gum polysaccharide).
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
The embodiment of the invention provides a preparation method of high-oxidation-resistance peach gum polysaccharide, which uses organic alkali to carry out nitrogen doping on the peach gum polysaccharide to obtain the high-oxidation-resistance peach gum polysaccharide.
In the embodiment of the invention, the organic base is an organic amine containing primary amine. The organic base selected by the invention is an organic compound containing amino in the molecule, and the organic base is an organic amine containing primary amine, so that the nitrogen atom on the primary amine has strong nucleophilicity and can react with peach gum polysaccharide more easily to realize nitrogen doping. Preferably, the organic base comprises one or more of ethylenediamine, diethylenetriamine and triethylenetetramine.
In the embodiment of the invention, the preparation method of the high-antioxidant peach gum polysaccharide specifically comprises the following steps:
crushing the dried natural crude peach gum into crude peach gum powder by using a crusher, adding deionized water and organic alkali at 20-35 ℃ for full swelling, stirring the swelled crude peach gum powder by using a stirrer to obtain peach gum suspension, placing the crude peach gum suspension into an oil bath pot for stirring, heating and hydrolyzing, putting the crude peach gum suspension into a dialysis bag for dialysis after the hydrolysis is finished, and freeze-drying after the dialysis is finished to obtain the high-antioxidant peach gum polysaccharide.
In a preferred embodiment of the present invention, the particle size of the crude peach gum powder is 30 mesh to 50 mesh. The size of the particle size of the crude peach gum powder directly influences the time required for swelling of the crude peach gum, and the swelling time is multiplied due to the excessive particle size. The particle size of the prepared crude peach gum powder is limited to the crusher equipment, the crusher in the laboratory can only crush the powder to the mesh, and in theory, the smaller the particle size, the faster the swelling, and the shorter the time required.
In the preferred embodiment of the invention, the volume ratio of the crude peach gum powder to the water to the organic alkali is 1:15-20:0.1-1.
In a preferred embodiment of the present invention, the swelling temperature is 20 to 35 ℃ (room temperature) and the swelling time is 4 to 8 hours. The swelling temperature is room temperature, and no redundant energy consumption is needed at the temperature, so that the preparation cost is reduced.
In a preferred embodiment of the present invention, the temperature of the oil bath hydrolysis is 90 to 110 ℃, preferably 95 to 110 ℃, the hydrolysis time of the oil bath hydrolysis is 2 to 8 hours, and the stirring speed is 1000 to 2000 rpm. The oil bath hydrolysis has the advantages that a stable working temperature and a higher temperature range are provided, the temperature condition required by polysaccharide hydrolysis can be quickly reached, the breakage of polysaccharide molecules is quickened, at high temperature, the sugar chains of the polysaccharide molecules can be broken to form smaller fragments or monosaccharides, meanwhile, carboxyl groups in the polysaccharide can be subjected to condensation reaction with organic alkali to form amide bonds, the temperature setting of the oil bath hydrolysis is the optimal parameter tested by experiments, under the condition, the hydrolysis speed of peach gum polysaccharide is increased, the carbonization of the peach gum polysaccharide can be caused due to the fact that the temperature is too high, and the hydrolysis degree of the peach gum polysaccharide is insufficient or the hydrolysis time is prolonged due to the fact that the temperature is too low. Too short hydrolysis time can cause excessive molecular weight of polysaccharide, which is unfavorable for water solubility and subsequent application, and after a certain hydrolysis time is reached, the molecular weight of peach gum polysaccharide tends to be stable, if the hydrolysis time is prolonged, the peach gum polysaccharide can be seriously degraded or even completely decomposed into small molecules, and the hydrolysis cost can be increased.
In the embodiment of the invention, the freezing temperature of the refrigerator is-4 to-24 ℃.
The natural crude peach gum used in the example of the present invention was picked in Gui Linyu mountain park in China, and ethylenediamine, diethylenetriamine and triethylenetetramine were purchased from the company of the chemical industry, inc.
The room temperature range in the embodiment of the invention is as follows: 20-35 ℃.
The technical scheme of the invention is further described by the following examples.
Example 1
(1) Crushing 1 kg of dried natural crude peach gum into 50-mesh peach gum powder by using a crusher, adding 20 times of deionized water and 0.1 time of ethylenediamine to swell at normal temperature, swelling at room temperature for 6 hours, and stirring by using a stirrer after swelling to obtain a peach gum suspension;
(2) Hydrolyzing the peach gum suspension obtained in the step (1) in an oil bath at 100 ℃, wherein the stirring speed is adjusted to 1500 rpm, and the hydrolysis time is 6 hours, so as to obtain a nitrogen-doped peach gum polysaccharide aqueous solution;
(3) And (3) putting the nitrogen-doped peach gum polysaccharide aqueous solution obtained in the step (2) into deionized water for dialysis for 48 hours, putting the water into a refrigerator for freezing for 24 hours after the dialysis is finished, and then, performing freeze drying to obtain the nitrogen-doped high-oxidation-resistance peach gum polysaccharide (in powder form).
The photograph of the nitrogen-doped high oxidation resistance peach gum polysaccharide prepared in the embodiment 1 of the present invention is shown in fig. 1, the photograph of the nitrogen-doped high oxidation resistance peach gum polysaccharide prepared in the embodiment 1 of the present invention after being dissolved in water is shown in fig. 2, and it can be seen from fig. 1 and fig. 2 that the nitrogen-doped high oxidation resistance peach gum polysaccharide has excellent water solubility.
The full spectrum of the X-ray photoelectron spectrum of the nitrogen-doped high oxidation resistance peach gum polysaccharide prepared in the embodiment 1 of the invention is shown in fig. 3, the spectrum of N1s is shown in fig. 4, and as can be seen from fig. 3 and fig. 4, the nitrogen doping is successfully realized in the hydrolysis process.
Example 2
(1) Crushing 1 kg of dried natural crude peach gum into 50-mesh peach gum powder by using a crusher, then adding 15 times of deionized water and 0.5 times of organic alkali ethylenediamine to swell at normal temperature, wherein the swelling is carried out at room temperature for 4 hours, and stirring by using a stirrer after swelling is finished to obtain a peach gum suspension;
(2) Hydrolyzing the peach gum suspension obtained in the step (1) in an oil bath at 95 ℃, wherein the stirring speed is adjusted to 1500 rpm, and the hydrolysis time is 6 hours, so as to obtain a nitrogen-doped peach gum polysaccharide aqueous solution;
(3) And (3) putting the nitrogen-doped peach gum polysaccharide aqueous solution obtained in the step (2) into deionized water for dialysis for 24 hours, putting the water into a refrigerator for freezing for 12 hours after the dialysis is finished, and then, performing freeze drying to obtain the nitrogen-doped high-oxidation-resistance peach gum polysaccharide (in powder form).
Example 3
(1) Crushing 1 kg of dried natural crude peach gum into 50-mesh peach gum powder by using a crusher, then adding 15 times of deionized water and 1 time of organic alkali ethylenediamine to swell at normal temperature, swelling at room temperature for 8 hours, and stirring by using a stirrer after swelling is finished to obtain a peach gum suspension;
(2) Hydrolyzing the peach gum suspension obtained in the step (1) in an oil bath at 100 ℃, wherein the stirring speed is adjusted to 1500 rpm, and the hydrolysis time is 8 hours, so as to obtain a nitrogen-doped peach gum polysaccharide aqueous solution;
(3) And (3) putting the nitrogen-doped peach gum polysaccharide aqueous solution obtained in the step (2) into deionized water for dialysis for 24 hours, putting the water into a refrigerator for freezing for 12 hours after the dialysis is finished, and then, performing freeze drying to obtain the nitrogen-doped high-oxidation-resistance peach gum polysaccharide (in powder form).
Example 4
(1) Crushing 1 kg of dried natural crude peach gum into 30-mesh peach gum powder by using a crusher, then adding 15 times of deionized water and 0.5 times of organic base triethylene tetramine for swelling at normal temperature, wherein the swelling is carried out at room temperature for 4 hours, and stirring by using a stirrer after swelling is finished to obtain a peach gum suspension;
(2) Hydrolyzing the peach gum suspension obtained in the step (1) in an oil bath at 97 ℃, wherein the stirring speed is 1300 rpm, and the hydrolysis time is 6 hours, so as to obtain a nitrogen-doped peach gum polysaccharide aqueous solution;
(3) And (3) putting the nitrogen-doped peach gum polysaccharide aqueous solution obtained in the step (2) into deionized water for dialysis for 48 hours, putting the water into a refrigerator for freezing for 24 hours after the dialysis is finished, and then, performing freeze drying to obtain the nitrogen-doped high-oxidation-resistance peach gum polysaccharide (in powder form).
Example 5
(1) Crushing 1 kg of dried natural crude peach gum into 30-mesh peach gum powder by using a crusher, then adding 20 times of deionized water and 0.5 times of organic base (diethylenetriamine and triethylenetetramine with the mass ratio of 1:1) to swell at normal temperature, wherein the swelling is carried out at room temperature for 8 hours, and stirring by using a stirrer after swelling is finished to obtain a peach gum suspension;
(2) Hydrolyzing the peach gum suspension obtained in the step (1) in an oil bath at 110 ℃, wherein the stirring speed is adjusted to 1000 rpm, and the hydrolysis time is 2 hours, so as to obtain a nitrogen-doped peach gum polysaccharide aqueous solution;
(3) And (3) putting the nitrogen-doped peach gum polysaccharide aqueous solution obtained in the step (2) into deionized water for dialysis for 48 hours, putting the water into a refrigerator for freezing for 24 hours after the dialysis is finished, and then, performing freeze drying to obtain the nitrogen-doped high-oxidation-resistance peach gum polysaccharide (in powder form).
Example 6
(1) Crushing 1 kg of dried natural crude peach gum into 30-mesh peach gum powder by using a crusher, then adding 15 times of deionized water and 1 time of organic base (mixed solution of ethylenediamine, diethylenetriamine and triethylenetetramine with the mass ratio of 1:1:1) to swell at normal temperature, wherein the swelling time is 6 hours, and stirring by using a stirrer after swelling is finished to obtain a peach gum suspension;
(2) Hydrolyzing the peach gum suspension obtained in the step (1) in an oil bath at 105 ℃, wherein the stirring speed is adjusted to 2000 rpm, and the hydrolysis time is 8 hours, so as to obtain a nitrogen-doped peach gum polysaccharide aqueous solution;
(3) And (3) putting the nitrogen-doped peach gum polysaccharide aqueous solution obtained in the step (2) into deionized water for dialysis for 24 hours, putting the water into a refrigerator for freezing for 24 hours after the dialysis is finished, and then, performing freeze drying to obtain the nitrogen-doped high-oxidation-resistance peach gum polysaccharide (in powder form).
Example 7
(1) Crushing 1 kg of dried natural crude peach gum into 50-mesh peach gum powder by using a crusher, then adding 15 times of deionized water and 0.8 times of organic base triethylene tetramine for swelling at normal temperature, carrying out swelling for 5 hours, and stirring by using a stirrer after swelling is finished to obtain a peach gum suspension;
(2) Hydrolyzing the peach gum suspension obtained in the step (1) in an oil bath at 110 ℃, wherein the stirring speed is adjusted to 1800 rpm, and the hydrolysis time is 8 hours, so as to obtain a nitrogen-doped peach gum polysaccharide aqueous solution;
(3) And (3) putting the nitrogen-doped peach gum polysaccharide aqueous solution obtained in the step (2) into deionized water for dialysis for 48 hours, putting the water into a refrigerator for freezing for 24 hours after the dialysis is finished, and then, performing freeze drying to obtain the nitrogen-doped high-oxidation-resistance peach gum polysaccharide (in powder form).
Comparative example 1
The only difference from example 1 is that no organic base is used for nitrogen doping, the specific preparation process is:
(1) Crushing 1 kg of dried natural crude peach gum into 50-mesh peach gum powder by using a crusher, adding deionized water with the volume of 20 times under normal temperature condition for swelling for 6 hours, and stirring by using a stirrer after swelling is finished to obtain peach gum suspension;
(2) Placing the peach gum suspension obtained in the step (1) into an oil bath pot at 100 ℃ for hydrolysis, wherein the stirring speed is adjusted to 1500 rpm, and the hydrolysis time is 6 hours, so as to obtain a peach gum polysaccharide aqueous solution;
(3) And (3) putting the nitrogen-doped peach gum polysaccharide aqueous solution obtained in the step (2) into deionized water for dialysis for 48 hours, putting into a refrigerator for freezing for 24 hours after the dialysis is finished, and then, freeze-drying to obtain the peach gum polysaccharide (powder).
Comparative example 2
The same as in example 1 was repeated except that the organic base was replaced by NaOH as an inorganic base having a concentration of 0.1mol/L for hydrolysis.
Comparative example 3
The difference from example 1 was only that 1 kg of dried natural crude peach gum was crushed into 100 mesh peach gum powder by a crusher.
Comparative example 4
The difference from example 1 is that 1 kg of dried natural crude peach gum is crushed into 50 mesh peach gum powder by a crusher, and then 25 times of deionized water and 0.5 times of inorganic alkali NaOH with concentration of 0.1mol/L are added to swell at normal temperature.
Comparative example 5
The difference from example 1 is only that the peach gum suspension obtained in step (1) is put into an oil bath at 150 ℃ for hydrolysis.
Comparative example 6
The difference from example 1 is only that the hydrolysis time in step (2) was 12 hours.
Comparative example 7
The difference from example 1 is only that the swelling time in step (1) is 12h.
Performance testing
The peach gum polysaccharide powder prepared in example 1 (nitrogen-doped peach gum polysaccharide) and comparative example 1 (undoped peach gum polysaccharide) was subjected to the 2, 2-diaza-di (3-ethyl-benzothiazole-6-sulfonic acid) diammonium salt) (ABTS) free radical clearance measurement according to the method of Yong Liu, yi-Qun Du, jun-Hui Wang, et al int.j. Biol. Macromol.2014,64,63-68, and the result is shown in fig. 5, and it can be seen from fig. 5 that the oxidation resistance of the peach gum polysaccharide after nitrogen doping by the method of the present invention is significantly enhanced.
The (ABTS) radical scavenging rate measurements for examples 2-7 and comparative examples 2-7 were as follows:
the nitrogen-doped peach gum polysaccharide prepared by example 2 had 25% clearance at 0.5mg/mL and reached 90% at 2 mg/mL. 50% clearance was achieved by the nitrogen-doped peach gum polysaccharide prepared in example 3 at a concentration of 0.5mg/mL, and almost 100% of the ABTS free radicals were removed at 1.5 mg/mL. The nitrogen-doped peach gum polysaccharide prepared in example 4 has a clearance effect of approximately 80% at a concentration of 1mg/mL, and a clearance efficiency of 100% at 1.5 mg/mL. The nitrogen-doped peach gum polysaccharide prepared in example 5 achieved 20% removal efficiency at a concentration of 0.5mg/mL and 80% removal efficiency at 2 mg/mL. The nitrogen-doped peach gum polysaccharide prepared by example 6 had a 90% removal efficiency at 1.5 mg/mL. The nitrogen-doped peach gum polysaccharide prepared by example 7 had a 95% removal efficiency at 1.5 mg/mL.
The ABTS radical scavenging efficiency of the inorganic base hydrolyzed peach gum polysaccharide prepared in comparative example 2 was lower than that of the nitrogen-doped peach gum polysaccharide of example 1, the nitrogen-doped peach gum polysaccharide of example 1 achieved almost 100% scavenging efficiency at a concentration of 2mg/mL, whereas the inorganic base hydrolyzed peach gum polysaccharide had only 15% scavenging efficiency in the scavenging effect of 2mg/mL, because the nitrogen-doped peach gum polysaccharide contained amino groups having a reducing property, which also had the effect of scavenging radicals.
In comparative example 3, the peach gum polysaccharide has poorer water solubility due to larger broken particle size, lower hydrolysis degree, small contact area with ABTS free radical, poorer scavenging effect, and only 60% scavenging efficiency at the concentration of 2 mg/mL.
In comparative example 4, more higher concentration NaOH was added in the swelling, but the ABTS radical scavenging effect on peach gum polysaccharide was not better, still only 15% scavenging efficiency at a concentration of 2 mg/mL.
In comparative example 5, peach gum polysaccharide was carbonized at a hydrolysis temperature of 150 ℃, was already partially insoluble in water, had reduced scavenging effect on ABTS free radicals, and had only 40% scavenging efficiency at a concentration of 2 mg/mL.
In comparative example 6, the prolonged hydrolysis time did not improve the removal effect nor the solubility, and the removal efficiency of nearly 100% was still achieved only at a concentration of 2 mg/mL.
In comparative example 7, the swelling time of the crude polysaccharide was prolonged, and similarly to the result of comparative example 6, the removal effect was not improved, the solubility was not improved, and the removal efficiency of nearly 100% could be achieved only at a concentration of 2 mg/mL.
The foregoing is merely a preferred embodiment of the present application, but the scope of the present application is not limited thereto, and any changes or substitutions easily conceivable by those skilled in the art within the technical scope of the present application should be covered in the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
Claims (10)
1. A preparation method of high-oxidation-resistance peach gum polysaccharide is characterized in that organic alkali is used for carrying out nitrogen doping on the peach gum polysaccharide to obtain the high-oxidation-resistance peach gum polysaccharide.
2. The method for preparing high antioxidant peach gum polysaccharide according to claim 1, wherein the organic base is an organic amine containing primary amine.
3. The method for preparing high-oxidation-resistance peach gum polysaccharide according to claim 2, wherein the organic base comprises one or more of ethylenediamine, diethylenetriamine and triethylenetetramine.
4. The method for preparing the high-oxidation-resistance peach gum polysaccharide according to claim 1, comprising the following steps:
crushing the crude peach gum into crude peach gum powder, adding water and organic alkali for swelling to obtain crude peach gum suspension, carrying out oil bath hydrolysis on the crude peach gum suspension, dialyzing and freeze-drying to obtain the high-oxidation-resistance peach gum polysaccharide.
5. The method for preparing high antioxidant peach gum polysaccharide according to claim 4, wherein the particle size of the crude peach gum powder is 30-50 mesh.
6. The method for preparing the high-oxidation-resistance peach gum polysaccharide according to claim 4, wherein the volume ratio of the crude peach gum powder to the water to the organic base is 1:15-20:0.1-1.
7. The method for preparing high antioxidant peach gum polysaccharide according to claim 4, wherein the swelling is performed at room temperature, and the swelling time is 4-8 hours.
8. The method for preparing high antioxidant peach gum polysaccharide according to claim 4, wherein the temperature of the oil bath hydrolysis is 90-110 ℃, the hydrolysis time of the oil bath hydrolysis is 2-8 hours, and the stirring speed of the oil bath hydrolysis is 1000-2000 rpm.
9. The peach gum polysaccharide with high oxidation resistance is characterized by being prepared by the preparation method according to any one of claims 1-8.
10. The use of the highly antioxidant peach gum polysaccharide according to claim 9 in the fields of cosmetics, functional foods and biomedical material preparation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311380715.XA CN117402266A (en) | 2023-10-24 | 2023-10-24 | Peach gum polysaccharide with high oxidation resistance and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311380715.XA CN117402266A (en) | 2023-10-24 | 2023-10-24 | Peach gum polysaccharide with high oxidation resistance and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117402266A true CN117402266A (en) | 2024-01-16 |
Family
ID=89495759
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311380715.XA Pending CN117402266A (en) | 2023-10-24 | 2023-10-24 | Peach gum polysaccharide with high oxidation resistance and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117402266A (en) |
-
2023
- 2023-10-24 CN CN202311380715.XA patent/CN117402266A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103059320A (en) | Solvent composition for dissolving chitin | |
| CN105646902B (en) | A kind of preparation method of iron-chitosan-metal supermolecular gel | |
| CN111253597B (en) | Chitin nanofiber/polyaniline composite gel film and preparation method thereof | |
| CN110746616A (en) | Cellulose hydrogel containing phenylboronic acid and preparation method and application thereof | |
| CN113372574B (en) | Polyvinyl alcohol hydrogel and preparation method thereof | |
| CN112661988B (en) | Preparation method of sodium alginate interpenetrating network hydrogel without ionic crosslinking | |
| CN111704728B (en) | Transparent ion-conductive cellulose hydrogel and preparation method and application thereof | |
| Zhang et al. | Facile production of chitin from shrimp shells using a deep eutectic solvent and acetic acid | |
| CN113045681A (en) | Enteromorpha polysaccharide hydrogel, preparation method and application in heavy metal pollution treatment | |
| CN101864082A (en) | Preparation method of chitin film | |
| CN105237644B (en) | A kind of cellulose with low degree and preparation method thereof | |
| CN117402266A (en) | Peach gum polysaccharide with high oxidation resistance and preparation method thereof | |
| CN116731365A (en) | High-strength, water-resistant and ultraviolet-resistant carboxymethyl cellulose/sodium alginate composite film and preparation method thereof | |
| CN115611996B (en) | Preparation method of regenerated chitin | |
| CN101381479A (en) | Method for synthesizing alkaline soluble glycol cellulose for spinning/membrane manufacturing | |
| CN108440812B (en) | Bioengineering rubber and preparation method thereof | |
| CN115594778B (en) | Method for extracting chitin by using acidic eutectic solvent | |
| CN109134701B (en) | Method for rapidly extracting high-purity low-molecular-weight chitin from shrimp and crab shells | |
| CN110408056A (en) | A kind of chitin hydrogel and preparation method thereof adulterating cellulose | |
| CN115478333B (en) | Antibacterial sakura fiber and preparation method thereof | |
| CN113150324B (en) | TEMPO oxidized Millettia speciosa champ cellulose/gellan gum pH response type hydrogel and preparation method and application thereof | |
| CN114272445B (en) | Hemostatic anti-adhesion material for use in vitro and in vivo and preparation method thereof | |
| CN113774091B (en) | Stable water-soluble nano-selenium and preparation method thereof | |
| CN112500583B (en) | Hydrophobically modified xanthan gum solution and preparation method and application thereof | |
| CN1235915C (en) | Fast degradation method of preparing molecular weight controllable chitosan |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |