CN112048084A - Preparation method of low-temperature crosslinked polyvinyl alcohol composite antibacterial peptide material - Google Patents
Preparation method of low-temperature crosslinked polyvinyl alcohol composite antibacterial peptide material Download PDFInfo
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- CN112048084A CN112048084A CN202010852084.7A CN202010852084A CN112048084A CN 112048084 A CN112048084 A CN 112048084A CN 202010852084 A CN202010852084 A CN 202010852084A CN 112048084 A CN112048084 A CN 112048084A
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- antibacterial peptide
- polyvinyl alcohol
- alcohol composite
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- 239000003910 polypeptide antibiotic agent Substances 0.000 title claims abstract description 85
- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 64
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 64
- 239000002131 composite material Substances 0.000 title claims abstract description 48
- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 21
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 14
- 239000007822 coupling agent Substances 0.000 claims description 13
- 125000003545 alkoxy group Chemical group 0.000 claims description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 7
- 239000003431 cross linking reagent Substances 0.000 claims description 7
- 230000009471 action Effects 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 4
- 239000003607 modifier Substances 0.000 claims description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000001580 bacterial effect Effects 0.000 description 6
- 241000222122 Candida albicans Species 0.000 description 5
- 241000191967 Staphylococcus aureus Species 0.000 description 5
- 241000194017 Streptococcus Species 0.000 description 5
- 229940095731 candida albicans Drugs 0.000 description 5
- 241000588724 Escherichia coli Species 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229920001817 Agar Polymers 0.000 description 2
- 239000001888 Peptone Substances 0.000 description 2
- 108010080698 Peptones Proteins 0.000 description 2
- 239000008272 agar Substances 0.000 description 2
- 235000015278 beef Nutrition 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 235000019319 peptone Nutrition 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
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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
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
-
- 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
- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
-
- 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
- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
Abstract
The invention belongs to the technical field of composite material production, and particularly relates to a preparation method of a low-temperature crosslinked polyvinyl alcohol composite antibacterial peptide material.
Description
Technical Field
The invention relates to the technical field of composite material production, in particular to a preparation method of a low-temperature crosslinked polyvinyl alcohol composite antibacterial peptide material.
Background
The polyvinyl alcohol is a polyhydroxy polymer, has good water solubility and high biocompatibility, is nontoxic and biodegradable to human bodies, and is widely applied to the fields of medical materials, food contact packaging materials and the like. The cationic antibacterial peptide is a micromolecular polypeptide with broad-spectrum antibacterial activity, has the positive charge and has the function of adsorbing pathogenic microorganisms (negative charge), so the cationic antibacterial peptide has the characteristics of quick sterilization, broad-spectrum antibacterial property, safety and effectiveness, and particularly attracts people's attention to the killing function of certain drug-resistant pathogenic bacteria. But the antibacterial peptide ions are sensitive and unstable, so that the application of the antibacterial peptide ions in the aspect of medicine is limited.
Disclosure of Invention
The invention aims to provide a preparation method of a low-temperature crosslinked polyvinyl alcohol composite antibacterial peptide material, which aims to solve the problems that the existing antibacterial peptide has poor cationic stability and an aminated PVA composite material has an antibacterial effect.
In order to achieve the purpose, the invention provides a preparation method of a low-temperature cross-linked polyvinyl alcohol composite antibacterial peptide material, which comprises the following steps:
the method comprises the following steps: the titanate coupling agent couples the hydroxyl of the polyvinyl alcohol with the carboxyl or hydroxyl of the antibacterial peptide through the alkoxy of the titanate coupling agent;
step two: polyvinyl alcohol and antibacterial peptide pass through under the action of titanate cross-linking agent
Forming the stable polyvinyl alcohol composite antibacterial peptide material.
Preferably, the pH value of the polyvinyl alcohol composite antibacterial peptide material is 5-6.
Preferably, the production temperature of the polyvinyl alcohol composite antibacterial peptide material is between 25 and 30 ℃.
Preferably, the concentration of the antibacterial peptide produced by the polyvinyl alcohol composite antibacterial peptide material is about 3604 ug/ml.
Preferably, the polyvinyl alcohol is used as a modifier of the antibacterial peptide, so that the stability of the antibacterial peptide is improved.
Preferably, the polyvinyl alcohol is used as a carrier of the antibacterial peptide, supports the antibacterial peptide and enables the antibacterial peptide to be uniformly dispersed.
Preferably, the polyvinyl alcohol and the antibacterial peptide are both polar materials, and compared with the prior art, the polyvinyl alcohol antibacterial peptide has good biocompatibility, and has the following beneficial effects:
through the common coordination of alkoxy in the titanate coupling agent, hydroxyl in polyvinyl alcohol, hydroxyl or carboxyl in the antibacterial peptide and the titanate cross-linking agent, the stability of the produced polyvinyl alcohol composite antibacterial peptide material is greatly improved, and the originally unavailable antibacterial effect is improved.
Drawings
FIG. 1 is a schematic view of the process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
Example (b):
referring to fig. 1, the present invention provides a technical solution: a preparation method of a low-temperature cross-linked polyvinyl alcohol composite antibacterial peptide material comprises the following steps:
the method comprises the following steps: the titanate coupling agent couples the hydroxyl of the polyvinyl alcohol with the carboxyl or hydroxyl of the antibacterial peptide through the alkoxy of the titanate coupling agent;
step two: polyvinyl alcohol and antibacterial peptide pass through under the action of titanate cross-linking agent
Forming the stable polyvinyl alcohol composite antibacterial peptide material.
The pH value of the polyvinyl alcohol composite antibacterial peptide material is 5-6;
the optimal temperature for producing the polyvinyl alcohol composite antibacterial peptide material is between 25 and 30 ℃;
the optimal concentration of the antibacterial peptide produced by the polyvinyl alcohol composite antibacterial peptide material is about 3604 ug/ml;
the polyvinyl alcohol can be used as a modifier of the antibacterial peptide, so that the stability of the antibacterial peptide is improved;
the polyvinyl alcohol can be used as a carrier of the antibacterial peptide, supports the antibacterial peptide and enables the antibacterial peptide to be uniformly dispersed;
the polyvinyl alcohol and the antibacterial peptide are both polar materials, and have good biocompatibility.
The first embodiment;
the preparation method of the polyvinyl alcohol composite antibacterial peptide material comprises the following specific steps;
s1: the titanate coupling agent couples the hydroxyl of the polyvinyl alcohol with the carboxyl or hydroxyl of the antibacterial peptide through the alkoxy of the titanate coupling agent;
polyvinyl alcohol and antibacterial peptide are put together under the action of titanate cross-linking agent, the pH value of production environment is set to 5, and the production temperature is set to 25 ℃.
S2: and (3) detecting the finally produced polyvinyl alcohol composite antibacterial peptide material, and detecting the antibacterial action of the aminated PVA composite material in the antibacterial peptide.
Example two;
the preparation method of the polyvinyl alcohol composite antibacterial peptide material comprises the following specific steps;
s1: the titanate coupling agent couples the hydroxyl of the polyvinyl alcohol with the carboxyl or hydroxyl of the antibacterial peptide through the alkoxy of the titanate coupling agent;
polyvinyl alcohol and antibacterial peptide are put together under the action of titanate cross-linking agent, the pH value of production environment is set to 5.5, and the production temperature is set to 27 ℃.
S2: and (3) detecting the finally produced polyvinyl alcohol composite antibacterial peptide material, and detecting the antibacterial action of the aminated PVA composite material in the antibacterial peptide.
Example three;
the preparation method of the polyvinyl alcohol composite antibacterial peptide material comprises the following specific steps;
s1: the titanate coupling agent couples the hydroxyl of the polyvinyl alcohol with the carboxyl or hydroxyl of the antibacterial peptide through the alkoxy of the titanate coupling agent;
polyvinyl alcohol and antibacterial peptide are put together under the action of titanate cross-linking agent, the pH value of production environment is set to 6, and the production temperature is set to 30 ℃.
S2: and (3) detecting the finally produced polyvinyl alcohol composite antibacterial peptide material, and detecting the antibacterial action of the aminated PVA composite material in the antibacterial peptide.
The experimental report of the antibacterial performance of the polyvinyl alcohol composite antibacterial peptide material comprises the following steps:
1. the purpose is as follows: and (3) detecting the antibacterial performance of the polyvinyl alcohol composite antibacterial peptide material.
2. Experimental materials, instruments: beef extract, peptone, sodium chloride (NaCl), agar, distilled water, 1.0mol/L NaOH solution, escherichia coli, staphylococcus aureus, streptococcus, candida albicans, a beaker, a culture dish, tweezers, an incubator, a pH meter, a pressure steam sterilization pot, a liquid transfer gun head and a test tube.
3. The experimental steps are as follows:
3.1 weighing beef extract (1.6g), peptone (1.2g), NaCl (0.8g), agar (3.0g) and dissolving in 100mL distilled water, heating to melt, adjusting pH to 7.3 with 1.0mol/L NaOH solution when the solution is cooled to room temperature, and autoclaving for about 30min to form the original sterile medium.
3.2 placing the polyvinyl alcohol composite antibacterial peptide material sample in a culture dish to prepare the antibacterial peptide material sample with the bacterial content of 5 multiplied by 105-10×106cfu/mL of bacterial suspension. Counting live bacteria of the bacterial liquid, adding colibacillus, staphylococcus aureus, streptococcus and candida albicans into the diluted liquid respectively, and cooling to form a solid culture medium. The plates inoculated with the bacteria were incubated at 37 ℃ for 48h, and the preliminary results were observed and continued on a sterile growth tube until day 7. Positive is indicated as (+) if the broth tube is turbid and the blood plate has bacteria growing; still clear as at day 7, considered sterile growth, indicated by (-). At the same time, a blank control set was set.
4. The experimental results are as follows: see tables 1-3 below.
Table 1 example a result of an experiment on antibacterial property of a polyvinyl alcohol composite antibacterial peptide material
| Bacterial strain | Day one | The next day | The third day | The fourth day | The fifth day | Day six | The seventh day |
| Escherichia coli | - | - | - | - | - | - | - |
| Staphylococcus aureus | - | - | - | - | - | - | - |
| Streptococcus sp | - | - | - | - | - | - | - |
| Candida albicans | - | - | - | - | - | - | - |
| Blank control group | + | + | + | + | + | + | + |
TABLE 2 Experimental results of antibacterial property of polyvinyl alcohol dimer composite antibacterial peptide material
| Bacterial strain | Day one | The next day | The third day | The fourth day | The fifth day | Day six | The seventh day |
| Escherichia coli | - | - | - | - | - | - | - |
| Staphylococcus aureus | - | - | - | - | - | - | - |
| Streptococcus sp | - | - | - | - | - | - | - |
| Candida albicans | - | - | - | - | - | - | - |
| Blank control group | + | + | + | + | + | + | + |
TABLE 3 experiment results of antibacterial property of composite antibacterial peptide material of trimeric vinyl alcohol in the example
| Bacterial strain | Day one | The next day | The third day | The fourth day | The fifth day | Day six | The seventh day |
| Escherichia coli | - | - | - | - | - | - | - |
| Staphylococcus aureus | - | - | - | - | - | - | - |
| Streptococcus sp | - | - | - | - | - | - | - |
| Candida albicans | - | - | - | - | - | - | - |
| Blank control group | + | + | + | + | + | + | + |
As can be seen from tables 1-3, the blank control group showed (+) property after 7 days of culture, while the 7 days of records of the four culture dishes containing the polyvinyl alcohol composite antibacterial peptide material showed (-) property, indicating that the synthesized titanate crosslinked polyvinyl alcohol composite antibacterial peptide material has good bactericidal effect. The result shows that the aminated PVA composite material has good bactericidal effect on the strains tested in the test, and has the characteristics of broad-spectrum antibiosis and strong-effect antibiosis.
While there have been shown and described the fundamental principles and essential features of the invention and advantages thereof, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof; the present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A preparation method of a low-temperature cross-linked polyvinyl alcohol composite antibacterial peptide material is characterized by comprising the following steps:
the method comprises the following steps: the titanate coupling agent couples the hydroxyl of the polyvinyl alcohol with the carboxyl or hydroxyl of the antibacterial peptide through the alkoxy of the titanate coupling agent;
step two: polyvinyl alcohol and antibacterial peptide pass through under the action of titanate cross-linking agent
Forming the stable polyvinyl alcohol composite antibacterial peptide material.
2. The preparation method of the low-temperature crosslinked polyvinyl alcohol composite antibacterial peptide material according to claim 1, characterized in that: the pH value of the polyvinyl alcohol composite antibacterial peptide material is 5-6.
3. The preparation method of the low-temperature crosslinked polyvinyl alcohol composite antibacterial peptide material according to claim 1, characterized in that: the production temperature of the polyvinyl alcohol composite antibacterial peptide material is between 25 and 30 ℃.
4. The preparation method of the low-temperature crosslinked polyvinyl alcohol composite antibacterial peptide material according to claim 1, characterized in that: the concentration of the antibacterial peptide produced by the polyvinyl alcohol composite antibacterial peptide material is about 3604 ug/ml.
5. The preparation method of the low-temperature crosslinked polyvinyl alcohol composite antibacterial peptide material according to claim 1, characterized in that: the polyvinyl alcohol is used as a modifier of the antibacterial peptide, and the stability of the antibacterial peptide is improved.
6. The preparation method of the low-temperature crosslinked polyvinyl alcohol composite antibacterial peptide material according to claim 1, characterized in that: the polyvinyl alcohol is used as a carrier of the antibacterial peptide, supports the antibacterial peptide and enables the antibacterial peptide to be uniformly dispersed.
7. The preparation method of the low-temperature crosslinked polyvinyl alcohol composite antibacterial peptide material according to claim 1, characterized in that: the polyvinyl alcohol and the antibacterial peptide are both polar materials, and have good biocompatibility.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113181422A (en) * | 2021-05-18 | 2021-07-30 | 四川轻化工大学 | Antibacterial nontoxic hydrogel dressing and preparation method thereof |
| CN117731817A (en) * | 2024-02-19 | 2024-03-22 | 浙江大学 | Preparation and application of coupled nano polypeptide HD5-myr antibacterial material |
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| CN117731817A (en) * | 2024-02-19 | 2024-03-22 | 浙江大学 | Preparation and application of coupled nano polypeptide HD5-myr antibacterial material |
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Inventor after: Fang Xiangming Inventor after: Wu Kangping Inventor after: Sun Yaqi Inventor after: Fan Longxue Inventor after: Cheng Baoli Inventor after: Xiong Qixing Inventor after: Lin Ru Inventor before: Wu Kangping |
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Application publication date: 20201208 |