CN115926258A - Cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol - Google Patents
Cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol Download PDFInfo
- Publication number
- CN115926258A CN115926258A CN202210712100.1A CN202210712100A CN115926258A CN 115926258 A CN115926258 A CN 115926258A CN 202210712100 A CN202210712100 A CN 202210712100A CN 115926258 A CN115926258 A CN 115926258A
- Authority
- CN
- China
- Prior art keywords
- menthol
- cellulose
- cyclodextrin
- zinc oxide
- composite material
- 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
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 239000000017 hydrogel Substances 0.000 title claims abstract description 76
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 title claims abstract description 72
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229940041616 menthol Drugs 0.000 title claims abstract description 72
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 48
- 229920002678 cellulose Polymers 0.000 title claims abstract description 44
- 239000001913 cellulose Substances 0.000 title claims abstract description 44
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 64
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 125000002091 cationic group Chemical group 0.000 claims abstract description 55
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims abstract description 34
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims abstract description 34
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 14
- 230000000694 effects Effects 0.000 claims abstract description 11
- 239000011159 matrix material Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 51
- 238000002360 preparation method Methods 0.000 claims description 30
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 10
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000001116 FEMA 4028 Substances 0.000 claims description 7
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 7
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 7
- 229960004853 betadex Drugs 0.000 claims description 7
- PUVAFTRIIUSGLK-UHFFFAOYSA-M trimethyl(oxiran-2-ylmethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC1CO1 PUVAFTRIIUSGLK-UHFFFAOYSA-M 0.000 claims description 6
- 230000001954 sterilising effect Effects 0.000 claims description 4
- 238000004659 sterilization and disinfection Methods 0.000 claims description 4
- 230000001965 increasing effect Effects 0.000 claims description 3
- 238000004132 cross linking Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 206010052428 Wound Diseases 0.000 abstract description 19
- 208000027418 Wounds and injury Diseases 0.000 abstract description 19
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 9
- 230000006870 function Effects 0.000 abstract description 4
- 230000029663 wound healing Effects 0.000 abstract description 3
- 230000000202 analgesic effect Effects 0.000 abstract description 2
- 230000003115 biocidal effect Effects 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 230000001139 anti-pruritic effect Effects 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 42
- 238000012360 testing method Methods 0.000 description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- 239000000523 sample Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 238000002474 experimental method Methods 0.000 description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 8
- 239000012153 distilled water Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 230000035699 permeability Effects 0.000 description 8
- 230000008961 swelling Effects 0.000 description 8
- 238000011068 loading method Methods 0.000 description 7
- 238000007619 statistical method Methods 0.000 description 7
- 230000002401 inhibitory effect Effects 0.000 description 6
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 239000003242 anti bacterial agent Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 239000003431 cross linking reagent Substances 0.000 description 4
- 230000001186 cumulative effect Effects 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000000284 extract Substances 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 238000004108 freeze drying Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000013641 positive control Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 241000588724 Escherichia coli Species 0.000 description 3
- 206010034133 Pathogen resistance Diseases 0.000 description 3
- 206010072170 Skin wound Diseases 0.000 description 3
- 239000000872 buffer Substances 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 210000004027 cell Anatomy 0.000 description 3
- 230000003833 cell viability Effects 0.000 description 3
- 231100000263 cytotoxicity test Toxicity 0.000 description 3
- 239000002609 medium Substances 0.000 description 3
- 239000013642 negative control Substances 0.000 description 3
- 238000005580 one pot reaction Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- FNBBXJWAHDKFDW-UHFFFAOYSA-J O[Zn](O)(O)O Chemical compound O[Zn](O)(O)O FNBBXJWAHDKFDW-UHFFFAOYSA-J 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000036592 analgesia Effects 0.000 description 2
- 230000001580 bacterial effect Effects 0.000 description 2
- 230000003385 bacteriostatic effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000502 dialysis Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000035876 healing Effects 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 206010002091 Anaesthesia Diseases 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 208000035143 Bacterial infection Diseases 0.000 description 1
- 229930186147 Cephalosporin Natural products 0.000 description 1
- 206010067482 No adverse event Diseases 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000037005 anaesthesia Effects 0.000 description 1
- 238000000540 analysis of variance Methods 0.000 description 1
- 230000000843 anti-fungal effect Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 229940124350 antibacterial drug Drugs 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 229940121375 antifungal agent Drugs 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229940041011 carbapenems Drugs 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000001768 cations Chemical group 0.000 description 1
- 238000004113 cell culture Methods 0.000 description 1
- 230000004663 cell proliferation Effects 0.000 description 1
- 229940124587 cephalosporin Drugs 0.000 description 1
- 150000001780 cephalosporins Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 238000002784 cytotoxicity assay Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 210000001339 epidermal cell Anatomy 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 210000002950 fibroblast Anatomy 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000003102 growth factor Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000003951 lactams Chemical class 0.000 description 1
- 210000000265 leukocyte Anatomy 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 231100000065 noncytotoxic Toxicity 0.000 description 1
- 230000002020 noncytotoxic effect Effects 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000006916 nutrient agar Substances 0.000 description 1
- 239000008363 phosphate buffer Substances 0.000 description 1
- 239000002504 physiological saline solution Substances 0.000 description 1
- 230000004983 pleiotropic effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- -1 preferably Substances 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000036560 skin regeneration Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 230000037314 wound repair Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention belongs to the technical field of composite cellulose materials, and relates to a cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol. The composite material takes hydroxyethyl cellulose as a matrix of hydrogel, and soluble cyclodextrin host molecules with cationic groups can be uniformly embedded into gaps of the cellulose material; menthol with antibacterial, analgesic and antipruritic effects is coated by cyclodextrin to increase water solubility and have slow release effect; the nanometer zinc oxide with the functions of antibiosis and promoting wound healing is adsorbed by cationic groups and is uniformly distributed on the surface of cellulose. The composite material has a huge application prospect in the field of wound dressings.
Description
Technical Field
The invention belongs to the technical field of composite cellulose materials, and relates to a cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol.
Background
For a long time, wounds such as burns and scalds are difficult to heal and are very painful for patients, and therefore, it is very important to develop a wound dressing having excellent performance and good effect. Traditional wound dressings, such as gauze and bandages, are single in function and may cause secondary damage to the wound surface when changing dressings. Modern novel wound dressings such as hydrogel, foam dressing, tissue engineering skin and intelligent dressing not only can resist external bacterial pollution, but also have multiple functions of moisturizing, promoting wound healing and the like, and are more and more widely applied. The hydrogel has a three-dimensional structure, good permeability and biocompatibility, can provide a moist environment for wound repair, overcomes the defects of the conventional dressing, and becomes an ideal candidate material for the dressing. Especially cellulose-based hydrogels, are receiving much attention and research due to their wide source, environmental friendliness and high biocompatibility. However, it is difficult to achieve antibacterial, analgesic and healing effects on wounds using only hydrogel. Therefore, there is an increasing search to combine functional molecules with hydrogels to produce hydrogel dressings with pleiotropic properties.
Currently most antibacterial agents are chemically modified natural compounds such as lactams, cephalosporins or carbapenems. However, with the widespread use and abuse of antibacterial drugs, the emergence of bacterial resistance has become a common phenomenon. In addition, the conventional antibacterial agents have disadvantages not only in the occurrence of bacterial resistance but also in their undesirable side effects. The use of large doses of antibiotics often results in intolerable toxicity. These have led to the development of alternative strategies for the treatment of bacterial diseases. Now, more and more researchers are focusing on metal nano antibacterial agents having high antibacterial efficiency and low bacterial resistance. The nano zinc oxide used in this study is one of the very widely studied metal particles used in antimicrobial wound dressings. Moreover, many studies have proved that nano zinc oxide is non-toxic to human body when applied to hydrogel wound dressings. However, metal nanoparticles are thermodynamically unstable and tend to aggregate to reduce their surface area. This aggregation affects their size, morphology, surface area and stability, resulting in a deterioration of antibacterial and antiviral properties. Thus, immobilization or stabilization of metal nanoparticles has become one of the potential methods to overcome the aggregation problem. Menthol is a naturally occurring organic substance, has the characteristics of cooling, analgesia, antibiosis, antifungal, anesthesia and permeability enhancement, and has no toxic effect on human bodies. However, small molecule menthol is very volatile in aqueous media, is very unstable, is not easily dissolved, can crystallize rapidly, and affects the shelf life of its application. Most importantly, menthol has a low solubility in water, which makes it difficult to disperse uniformly in conventional drug delivery systems.
Therefore, how to ensure the uniform loading of nano zinc oxide on cellulose and improve the water solubility of menthol are key problems to be solved. Because it is the key point for preparing the cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol.
Disclosure of Invention
One objective of the invention is to provide a cellulose-based hydrogel composite loaded with nano zinc oxide and menthol; the invention also aims to provide a preparation method of the cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol. The invention also aims to provide the application of the cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol in skin wound dressings.
The purpose of the invention is realized by the following technical scheme:
in one aspect, the invention provides a cellulose-based hydrogel composite loaded with nano zinc oxide and menthol, which takes hydroxyethyl cellulose as a matrix of the hydrogel, and cyclodextrin with cationic groups is uniformly embedded into gaps of the cellulose material; the menthol is coated by the cyclodextrin, so that the water solubility is increased and the slow release effect is achieved; .
In the composite material, preferably, the cellulose is hydroxyethyl cellulose; the cyclodextrin is beta-cyclodextrin modified by quaternary ammonium salt; the nano zinc oxide is generated in situ by zinc nitrate hexahydrate; the menthol is rod-shaped menthol crystal with purity higher than 98%.
Under the condition of lower magnification, the surface of the hydrogel of the cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol can still see a sharp quasi-crystalline layer formed by the cationic cyclodextrin adhered on the surface of the hydrogel, so that a smooth and ordered tight combination form is formed. The pores of the hydrogel are large and not blocked by nano zinc oxide, which increases the air permeability. The size of the zinc oxide is 20-100 nm and reaches the nanometer level. The fiber composite material with the special structure can be widely applied to the field of skin wound dressings.
On the other hand, the invention also provides a preparation method of the cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol, which comprises the following steps:
mixing beta-cyclodextrin and 2, 3-epoxypropyl trimethyl ammonium chloride, heating and stirring to obtain cationic cyclodextrin;
adding menthol into a water solution of cationic cyclodextrin, and stirring to obtain a cyclodextrin inclusion compound;
under the condition of strong alkalinity, adding cyclodextrin inclusion compound solution dissolved with zinc nitrate hexahydrate into hydroxyethyl cellulose solution, and then adding epichlorohydrin for crosslinking. Heating the obtained hydrogel to obtain the cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol.
The invention adopts a one-pot reaction. Hydroxyethyl cellulose can be crosslinked into hydrogel with three-dimensional network by epichlorohydrin in alkaline environment, and meanwhile, the cationic cyclodextrin wrapping menthol can be uniformly embedded into the grid of the hydrogel; zinc nitrate hexahydrate becomes negatively charged tetrahydroxy zinc ions in a strong alkaline environment, is combined with cationic cyclodextrin to be uniformly distributed in hydrogel, and is further heated to generate nano zinc oxide in situ; finally obtaining a cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol; the composite material has good biocompatibility, mechanical property and water absorption property, and has great application prospect in the field of wound dressings.
In the preparation method, the proportion of the hydroxyethyl cellulose and the epichlorohydrin is adjusted according to actual requirements on the basis of reaching the maximum mechanical strength.
In the above preparation method, preferably, the mass ratio of the cationic cyclodextrin to the hydroxyethyl cellulose is (5-10) to 1.
In the preparation method, the carrying amount of the menthol is regulated according to actual requirements by taking the maximum inclusion amount of the cationic cyclodextrin as a standard.
In the preparation method, the hydroxyethyl cellulose is dispersed in pure water to prepare the hydroxyethyl cellulose aqueous solution, wherein the solid content of the hydroxyethyl cellulose aqueous solution is 3-5 wt%.
In the preparation method, the dispersion method of the inclusion menthol cationic cyclodextrin is to dissolve the inclusion menthol cationic cyclodextrin in a sodium hydroxide solution, and the concentration of the sodium hydroxide solution is adjusted according to actual needs.
In the preparation method, the addition amount of the zinc nitrate hexahydrate is adjusted according to the actual performance of the material.
In the prior art, cyclodextrin aqueous solution and hydroxyethyl cellulose solution are directly mixed, and cyclodextrin can be uniformly embedded in a cellulose grid after being crosslinked into hydrogel. This greatly improves the mechanical properties of the hydrogel and allows the material surface to assume a smooth and ordered morphology.
In the above production method, the temperature for the heat treatment is preferably 60 to 80 ℃ and the time for the heat treatment is preferably 10 to 12 hours. Under the heating condition, the tetrahydroxy zinc ions with negative charges gradually become nano-scale zinc oxide particles; the nanometer zinc oxide is further coordinated with cation groups on the cyclodextrin and hydroxyl groups on the cellulose in situ to be firmly adsorbed on the cellulose. The nano zinc oxide is spherical particles, the diameter range of the particles is 20-100 nm, and the nano zinc oxide is uniformly distributed on the surface of cellulose.
In the above preparation method, preferably, the sterilization temperature is 121 ℃; the time is 15-18 min; the pressure was 0.12MPa. Sterilization is a process necessary to make medical materials into end products.
In another aspect, the invention also provides an application of the cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol in preparation of a skin wound dressing.
The invention has the beneficial effects that:
(1) The invention adopts a one-pot reaction. Hydroxyethyl cellulose can be crosslinked into hydrogel with three-dimensional network by epichlorohydrin under alkaline environment, and the cationic cyclodextrin wrapping menthol can be uniformly embedded into the grid of the hydrogel; zinc nitrate hexahydrate becomes negatively charged zinc ions with tetrahydroxy groups in a strong alkaline environment, the zinc ions are combined with cationic cyclodextrin and uniformly distributed in hydrogel, and the nano zinc oxide is further generated in situ by heating; finally obtaining a cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol; the composite material has good biocompatibility, mechanical property and water absorption property, and has great application prospect in the field of wound dressings.
(2) The invention adopts one-pot reaction, has simple preparation method and no by-product. The nano zinc oxide adopts an in-situ generation method, has mild preparation conditions, is stably loaded on a cellulose substrate, is uniformly dispersed and does not aggregate. The menthol is included by the cationic cyclodextrin, so that the loading capacity is greatly improved, and the slow release effect is realized. The composite material has great application prospect in the aspects of providing multiple effects of analgesia, sterilization, wound healing promotion and the like for the novel wound dressing.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
The implementation provides a preparation method of a cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol, which comprises the following steps:
(1) Preparation of cationic cyclodextrin:
the water content of the system was 20.2wt%. The amounts of the sodium hydroxide catalyst, the accelerator absolute ethyl alcohol and the cationic etherifying agent (2, 3-epoxypropyltrimethylammonium chloride) were 2.4wt%, 5.0wt% and 64.7wt%, respectively, relative to the mass percentage of the cationic cyclodextrin. Under 70 ℃ oil bath, the beta-cyclodextrin and the cationic etherifying agent are added into the sodium hydroxide solution at the same time. After the solution is stirred for 4 hours, excess ethanol is poured in, and washing is carried out for 3 to 4 times. The filtered solid was dried in an oven at 40 ℃ and ground to a powder.
(2) Preparing a menthol/cationic cyclodextrin inclusion compound:
menthol and cationic cyclodextrin were added to a flask containing 0.45mol/L of an aqueous solution of cationic cyclodextrin at a molar ratio of 1. The solution was magnetically stirred at room temperature for 6h and then filtered. The filtrate was freeze-dried to obtain a clathrate solid.
(3) Preparation of an aqueous solution of hydroxyethyl cellulose:
dissolving hydroxyethyl cellulose powder in pure water and stirring the solution until the solution is uniform to prepare a hydroxyethyl cellulose solution with the solid content of 5wt%.
(4) Preparation of hydrogel:
first, 2.5g of the above menthol/cationic cyclodextrin inclusion compound and 0.2g of zinc nitrate hexahydrate were dissolved in 5.0mL of a 20wt% sodium hydroxide solution. After stirring for 10 minutes, 6.0mL of the above hydroxyethylcellulose solution was added. The solution was transferred to a 25.0mL flat bottom beaker and stirred for 40min. Then, 3.5mL of epichlorohydrin was added to the solution, and the mixture was stirred for 15min. Sealed and left for 8 hours. Finally, they are stored in an oven and treated for 12 hours at 80 ℃ to convert the zinc ions of tetrahydroxy group into nano zinc oxide. The material was dialyzed by immersing in excess distilled water to remove excess base, cross-linking agent and other soluble polymers. After about one day, the cellulose-based hydrogel composite loaded with nano zinc oxide and menthol is obtained by freeze drying.
Example 2
The embodiment provides a preparation method of a cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol, which comprises the following steps:
(1) Preparation of cationic cyclodextrin:
the water content of the system was 20.2wt%. The amounts of the sodium hydroxide catalyst, the accelerator absolute ethyl alcohol and the cationic etherifying agent (2, 3-epoxypropyltrimethylammonium chloride) were 2.4wt%, 5.0wt% and 64.7wt%, respectively, relative to the mass percentage of the cationic cyclodextrin. Under 70 ℃ oil bath, the beta-cyclodextrin and the cationic etherifying agent are added into the sodium hydroxide solution at the same time. After the solution was stirred for 4 hours, excess ethanol was poured in and washed 3-4 times. The filtered solid was dried in an oven at 40 ℃ and ground to a powder.
(2) Preparing a menthol/cationic cyclodextrin inclusion compound:
menthol and cationic cyclodextrin were added to a flask containing 0.45mol/L of an aqueous solution of cationic cyclodextrin at a molar ratio of 1. The solution was magnetically stirred at room temperature for 6h and then filtered. The filtrate was freeze-dried to obtain a clathrate solid.
(3) Preparation of an aqueous solution of hydroxyethyl cellulose:
dissolving the hydroxyethyl cellulose powder in pure water and stirring the solution until the solution is uniform to prepare the hydroxyethyl cellulose solution with the solid content of 5wt%.
(4) Preparation of hydrogel:
first, 2.5g of the above menthol/cationic cyclodextrin inclusion compound and 0.4g of zinc nitrate hexahydrate were dissolved in 5.0mL of 28wt% sodium hydroxide solution. After stirring for 10 minutes, 6.0mL of the above hydroxyethylcellulose solution was added. The solution was transferred to a 25.0mL flat bottom beaker and stirred for 40min. Then, 3.5mL of epichlorohydrin was added to the solution, and the mixture was stirred for 15min. Sealed and left for 8 hours. Finally, the zinc oxide particles are stored in an oven and treated for 12 hours at 80 ℃ to convert the zinc tetrahydroxy ions into nano zinc oxide. The material was dialyzed by immersing in excess distilled water to remove excess base, cross-linking agent and other soluble polymers. After about one day, the cellulose-based hydrogel composite loaded with nano zinc oxide and menthol is obtained by freeze drying.
Example 3
The implementation provides a cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol, which comprises the following steps:
(1) Preparation of cationic cyclodextrin:
the water content of the system was 20.2wt%. The amounts of the sodium hydroxide catalyst, the accelerator absolute ethyl alcohol and the cationic etherifying agent (2, 3-epoxypropyltrimethylammonium chloride) were 2.4wt%, 5.0wt% and 64.7wt%, respectively, relative to the mass percentage of the cationic cyclodextrin. Under 70 ℃ oil bath, the beta-cyclodextrin and the cationic etherifying agent are added into the sodium hydroxide solution at the same time. After the solution was stirred for 4 hours, excess ethanol was poured in and washed 3-4 times. The filtered solid was dried in an oven at 40 ℃ and ground to a powder.
(2) Preparing a menthol/cationic cyclodextrin inclusion compound:
menthol and cationic cyclodextrin were added to a flask containing 0.45mol/L of an aqueous solution of cationic cyclodextrin at a molar ratio of 1. The solution was magnetically stirred at room temperature for 6h and then filtered. The filtrate was freeze-dried to obtain a clathrate solid.
(3) Preparation of an aqueous solution of hydroxyethyl cellulose:
dissolving hydroxyethyl cellulose powder in pure water and stirring the solution until the solution is uniform to prepare a hydroxyethyl cellulose solution with the solid content of 5wt%.
(4) Preparation of hydrogel:
first, 2.5g of the above menthol/cationic cyclodextrin inclusion compound and 0.6g of zinc nitrate hexahydrate were dissolved in 5.0mL of 34wt% sodium hydroxide solution. After stirring for 10 minutes, 6.0mL of the above hydroxyethylcellulose solution was added. The solution was transferred to a 25.0mL flat bottom beaker and stirred for 40min. Then, 3.5mL of epichlorohydrin was added to the solution, and the mixture was stirred for 15min. Sealed and left for 8 hours. Finally, they are stored in an oven and treated for 12 hours at 80 ℃ to convert the zinc ions of tetrahydroxy group into nano zinc oxide. The material was dialyzed by immersing in excess distilled water to remove excess base, cross-linking agent and other soluble polymers. After about one day, the cellulose-based hydrogel composite loaded with nano zinc oxide and menthol is obtained by freeze drying.
Comparative example
The implementation provides a preparation method of a cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol, which comprises the following steps:
(1) Preparation of cationic cyclodextrin:
the water content of the system was 20.2wt%. The amounts of the sodium hydroxide catalyst, the accelerator absolute ethyl alcohol and the cationic etherifying agent (2, 3-epoxypropyltrimethylammonium chloride) were 2.4wt%, 5.0wt% and 64.7wt%, respectively, relative to the mass percentage of the cationic cyclodextrin. Under 70 ℃ oil bath, the beta-cyclodextrin and the cationic etherifying agent are added into the sodium hydroxide solution at the same time. After the solution was stirred for 4 hours, excess ethanol was poured in and washed 3-4 times. The filtered solid was dried in an oven at 40 ℃ and ground to a powder.
(2) Preparing the menthol/cationic cyclodextrin inclusion compound:
menthol and cationic cyclodextrin were added to a flask containing 0.45mol/L of an aqueous solution of cationic cyclodextrin at a molar ratio of 1. The solution was magnetically stirred at room temperature for 6h and then filtered. The filtrate was freeze-dried to obtain a clathrate solid.
(3) Preparation of an aqueous solution of hydroxyethyl cellulose:
dissolving the hydroxyethyl cellulose powder in pure water and stirring the solution until the solution is uniform to prepare the hydroxyethyl cellulose solution with the solid content of 5wt%.
(4) Preparation of hydrogel:
first, 2.5g of the above menthol/cationic cyclodextrin inclusion compound was dissolved in 5.0mL of 10wt% sodium hydroxide solution. After stirring for 10 minutes, 6.0mL of the above hydroxyethylcellulose solution was added. The solution was transferred to a 25.0mL flat bottom beaker and stirred for 40min. Then, 3.5mL of epichlorohydrin was added to the solution, and the mixture was stirred for 15min. Sealed and left for 8 hours. Finally, they are stored in an oven and treated for 12 hours at 80 ℃ to convert the zinc ions of tetrahydroxy group into nano zinc oxide. The material was dialyzed by immersing in excess distilled water to remove excess base, cross-linking agent and other soluble polymers. After about one day, the cellulose-based hydrogel composite loaded with nano zinc oxide and menthol is obtained by freeze drying.
Mechanical property test experiment
Mechanical property tests were performed on examples 1, 2,3 and comparative examples, as follows:
the mechanical properties of the hydrogels were estimated by an Edeberg push-pull dynamometer (Jiangsu Zhongning, china, science and technology Co., ltd.). The prepared hydrogel dressing was cut into the same shape and size (2 cm long, 2 cm wide, 3 cm high) and placed in a separate 15.0mL flask. The hydrogel was pressed vertically downward with a 15cm diameter probe on a push-pull gauge and the maximum pressure it can withstand was obtained at its slow speed. The experiments were performed in triplicate and statistical analysis was performed.
The specific test results are shown in the following table 1: mechanical properties of example 1, example 2, example 3 and comparative example composites
As can be seen from the tests of example 1, example 2, example 3 and comparative example, these results indicate that the loading of nano-zinc oxide increases the mechanical strength of the hydrogel, which means that these hydrogel films can withstand sufficient pressure to provide effective protection to the wound during daily activities.
Swelling Performance test experiment
The swelling performance test was performed on examples 1, 2,3 and comparative examples, as follows:
the swelling behavior of the hydrogel in PBS solution was measured by weighing. The samples were immersed in phosphate buffer at pH 7.4 and periodically removed. The water attached to the surface was carefully absorbed with filter paper and their mass was accurately weighed until the gel mass reached equilibrium. The experiments were performed in triplicate and statistical analysis was performed.
The swelling degree calculation formula is as follows: q = (w) t -w 0 )/w 0 Wherein w is 0 Is the initial mass of the sample, w t Is the mass of the sample that achieves the maximum swelling degree.
The specific test results are shown in the following table 2: comparison of swelling Performance of example 1, example 2, example 3 and comparative example composites
For the first time | For the second time | The third time | Mean value of | |
Example 1 | 38.3185 | 39.7197 | 38.6383 | 38.89214 |
Example 2 | 32.3590 | 33.4958 | 31.8160 | 32.55691 |
Example 3 | 22.0751 | 23.1841 | 21.8181 | 22.35911 |
Comparative example | 41.0353 | 42.1873 | 40.7693 | 41.33063 |
By testing examples 1, 2,3 and comparative examples, it can be seen that the higher the loading of nano zinc oxide, the lower the degree of swelling. However, as a wound dressing, the degree of swelling should not be too high to avoid compression of the wound. The sample of example 3 has the best swelling properties here.
Water retention property test experiment
The water retention performance tests of example 1, example 2, example 3 and comparative example were carried out, and are specifically as follows:
the water-imbibed sample was weighed and placed at a temperature of 25 ℃ and a humidity of 35%. The mass was measured periodically while calculating the water loss rate. The experiments were performed in triplicate and statistical analysis was performed.
The water loss rate calculation formula is as follows: p = (w) 0 -w t )/w 0 X 100% where w 0 Is the initial mass of the hydrogel, w t Is the final constant mass of the sample.
The specific test results are shown in the following table 3: comparison of Water holding Properties of example 1, example 2, example 3 and comparative example composites
By testing example 1, example 2, example 3 and comparative example, it can be known that the loading of nano zinc oxide helps to increase the water retention capacity of the hydrogel dressing. The wound dressing with good water retention property is beneficial to releasing growth factors, accelerating cell proliferation, improving the mobility of epidermal cells and enhancing the function of white blood cells. The sample of example 3 has the best water retention properties here.
Oxygen permeability test experiment
The oxygen permeability test was performed on example 3 alone, as follows:
the flask was filled with 300mL of distilled water cooled after boiling, and the mouth of the flask was sealed with a hydrogel film. The oxygen permeation of the hydrogel was measured over 4 hours, 8 hours and 12 hours, respectively, and an open bottle was set as a control. Under the same conditions, distilled water which is not boiled for deoxidation for a long time is used as a positive control, and distilled water which is just boiled for deoxidation is used as a negative control. The experiments were performed in parallel five times and subjected to statistical analysis.
The oxygen permeability of the hydrogel was determined by measuring the oxygen content of the water in the flask using the winkler method.
The specific test results are shown in the following table 4: oxygen permeability of the composite of example 3
As can be seen from the oxygen permeability test of the embodiment 3, the prepared hydrogel dressing can ensure the permeation of a large amount of oxygen and promote the healing of wounds.
Antibacterial property test experiment
The antibacterial performance tests of example 1, example 2, example 3 and comparative example were carried out, and the details are as follows:
the antibacterial activity of the prepared hydrogel composite material is measured by an oxford ring diffusion method. For this purpose, gram-negative E.coli and gram-positive S.aureus bacteria were used. The diluted bacterial suspensions were inoculated and spread separately on sterilized nutrient agar medium. The hydrogel sample was added to the oxford ring and placed on the medium. Culturing for 18-20 h in a thermostat at 37 ℃. And observing the bacteriostatic ability of the sample through the size of the inhibition zone. The experiments were performed in triplicate and statistical analysis was performed.
The specific test results are shown in the following table 5: the specific test results are shown in the following table 3: comparison of antibacterial Properties of example 1, example 2, example 3 and comparative example composites
Compared with a comparative example, the antibacterial effect of the hydrogel dressing can be greatly enhanced by the loading of the nano zinc oxide. The bacteriostatic diameters of the samples of example 1, example 2 and example 3 did not change regularly. The sample of example 2 showed the best inhibitory effect against E.coli and the worst inhibitory effect against S.aureus. The sample of example 3 showed the best inhibitory effect against Staphylococcus aureus and the worst inhibitory effect against Escherichia coli. However, the loading of nano-zinc oxide formed in this range did not produce an excessive difference in the inhibitory effect of the hydrogel dressing. Therefore, it is considered that the inhibitory effects of the samples of example 1, example 2 and example 3 are not significantly different.
Test experiment for slow release effect of hydrogel dressing on menthol
The sustained release effect test was performed on example 3 alone, as shown below:
the effect of menthol release from the hydrogel dressing over 10 hours was investigated using dialysis bag diffusion technology. 5.0g of the lyophilized sample was filled in a dialysis bag, then 20.0mL of distilled water was added, both ends were clamped with a clamp, and finally, 200mL of PBS buffer was immersed. Seal agitation was performed at 37 ℃ at a speed of 350 rpm. 2.0mL of released PBS buffer was taken every hour, while 2.0mL of fresh PBS buffer was added. The amount of menthol released was determined by gas chromatography. The experiments were performed in triplicate and statistical analysis was performed.
Cumulative release efficiency calculation formula of menthol:
r = (cumulative amount of menthol released after specified time)/(total amount of menthol released within 10 hours) × 100%
The specific test results are shown in table 6 below: 10 hour cumulative release efficiency change of menthol in the composite of example 3
For the first time (%) | Second time (%) | Third time (%) | Average (%) | |
0 | 0 | 0 | 0 | 0 |
1h | 21.4789 | 20.7747 | 21.4789 | 21.24413 |
2h | 25.9507 | 26.0563 | 26.0563 | 26.02113 |
3h | 31.7958 | 31.6901 | 32.3944 | 31.96009 |
4h | 35.9155 | 34.8592 | 34.5070 | 35.0939 |
5h | 40.7394 | 40.4930 | 40.8451 | 40.69249 |
6h | 44.4718 | 42.9578 | 42.9578 | 43.46244 |
7h | 52.817 | 52.1127 | 55.634 | 53.52113 |
8h | 63.2747 | 66.1268 | 60.3944 | 63.26526 |
9h | 84.7183 | 85.0423 | 89.9578 | 86.57277 |
10h | 100.000 | 106.1549 | 99.0704 | 101.74178 |
Fitting by substituting numerical value to obtain M t /M ∞ =0.0014t +0.0395, wherein M t /M ∞ Is the cumulative release efficiency of menthol over a time interval t (min), 0.0014 is the constant release rate of the kinetic model. 0.0395 is the intercept of this equation.
The analysis of variance results for the kinetic model, "Prob > F", were below 0.05, indicating that the fitted curve in the experimental design was statistically significant at a 95% confidence level.
This indicates that menthol can be released at a nearly constant rate. A constant menthol release rate reduces fluctuations in menthol concentration and increases the adaptability of the wound to menthol.
Test for toxicity of sample
Cytotoxicity tests were performed on example 3 alone, as shown below:
in vitro cytotoxicity assays were performed by the MTT method.
The sample is first sterilized. Then, 0.1g of the hydrogel was extracted with physiological saline according to ISO 10993-5 to prepare extracts (0, 200mg/mL, 40mg/mL, 80mg/mL and 160 mg/mL) at different concentrations. Cytotoxicity tests were performed using the extract.
In each well of a 96-well plate, 10 was placed 4 Fibroblasts (L929) were cultured for 24 hours (carbon dioxide pressure 5%, humidity 98%, temperature 37 ℃). The same cells were divided into two groups: (1) Negative control (L929 cells) and (2) positive control (hydrogel extract was directly added to the medium), 20. Mu.L of 5mg/mL MTT solution was added to each well after 24 hours and 48 hours of total incubation. After 4 hours of cell culture, carefully remove all liquid from the wells and add 150 μ L of dimethyl sulfoxide. Shake for 15 seconds to ensure complete dissolution of the precipitate. Finally, byThe microplate reader measures the absorbance value at 490 nm. The experiments were performed in triplicate and statistical analysis was performed.
Cell viability = [ OD (sample) -OD (positive control) ]/[ OD (negative control) -OD (positive control) ] × 100%
The specific test results are shown in table 7 below: cell viability at 24 and 48 hours after addition of different concentrations of the extract of the composite material of example 3
According to GB/T16886.5-2003 (ISO 10993-5 1999), samples with a cell viability of more than 75% are considered to be non-cytotoxic. This indicates that the synthetic hydrogel dressing did not affect the growth of these cells. The results show that all the prepared hydrogel dressings can be used as wound dressings for skin regeneration.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (10)
1. A cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol, wherein the nano zinc oxide in the composite material is uniformly distributed on the surface of cellulose; menthol is encapsulated by cyclodextrin and carried into the material.
2. The nano-zinc oxide and menthol-loaded cellulose-based hydrogel composite according to claim 1, wherein hydroxyethyl cellulose is used as a matrix of the composite; the cyclodextrin with the cationic group is uniformly embedded into the gaps of the cellulose composite material; the menthol is coated by the cyclodextrin, so that the water solubility is increased and the slow release effect is achieved; the nano zinc oxide is adsorbed by cationic groups and uniformly distributed on the surface of the cellulose.
3. The method for preparing the nano zinc oxide and menthol-loaded cellulose-based hydrogel composite material according to claim 1 or 2, which comprises the following steps:
mixing beta-cyclodextrin and 2, 3-epoxypropyl trimethyl ammonium chloride, heating and stirring to obtain cationic cyclodextrin;
adding menthol into an aqueous solution of cationic cyclodextrin, and stirring to obtain a cyclodextrin inclusion compound;
under the condition of strong alkalinity, adding cyclodextrin inclusion compound solution dissolved with zinc nitrate hexahydrate into hydroxyethyl cellulose solution, and then adding epichlorohydrin for crosslinking. Heating the obtained hydrogel to obtain the cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol.
4. The process according to claim 3, wherein the proportions of hydroxyethylcellulose and of epichlorohydrin are adjusted according to the actual requirements, on the basis of reaching maximum mechanical strength.
5. The preparation method of claim 3, wherein the mass ratio of the cationic cyclodextrin to the hydroxyethyl cellulose is (5-10) to 1.
6. The method of claim 3, wherein the carrying amount of menthol is adjusted by actual need based on the maximum inclusion amount of the cationic cyclodextrin.
7. The preparation method of claim 3, wherein the hydroxyethyl cellulose is dispersed by dissolving in pure water to obtain an aqueous solution of hydroxyethyl cellulose with a solid content of 3-5 wt%; the dispersion method of the cationic cyclodextrin including menthol is to dissolve the cationic cyclodextrin in an aqueous solution, and the concentration of the aqueous solution is adjusted according to actual needs.
8. The production method according to claim 3, wherein the amount of zinc nitrate hexahydrate added is adjusted according to the actual properties of the material.
9. The method according to claim 3, wherein the heating is preferably carried out at a temperature of 60 to 80 ℃ for 10 to 12 hours.
Preferably, the sterilization temperature is 121 ℃; the time is 15-18 min; the pressure was 0.12MPa.
10. Use of the nano zinc oxide and menthol-loaded cellulose-based hydrogel composite according to claim 1 or 2 in the preparation of a skin repair dressing.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210712100.1A CN115926258A (en) | 2022-06-22 | 2022-06-22 | Cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210712100.1A CN115926258A (en) | 2022-06-22 | 2022-06-22 | Cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol |
Publications (1)
Publication Number | Publication Date |
---|---|
CN115926258A true CN115926258A (en) | 2023-04-07 |
Family
ID=86649583
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210712100.1A Pending CN115926258A (en) | 2022-06-22 | 2022-06-22 | Cellulose-based hydrogel composite material loaded with nano zinc oxide and menthol |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN115926258A (en) |
-
2022
- 2022-06-22 CN CN202210712100.1A patent/CN115926258A/en active Pending
Non-Patent Citations (1)
Title |
---|
JIANG, LH 等: "Preparation and study of cellulose-based ZnO NPs@HEC/C-β-CD/Menthol hydrogel as wound dressing", BIOCHEMICAL ENGINEERING JOURNAL, vol. 184, pages 108488 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Ye et al. | Construction of cellulose/nanosilver sponge materials and their antibacterial activities for infected wounds healing | |
CN110354295B (en) | Photo-thermal conversion material and preparation method thereof | |
CN111154149A (en) | Hydrogel and preparation method and dressing thereof | |
CN101664563B (en) | Preparation method of anti-bacterial hydrogel dressing | |
Ahmed et al. | Enhancing the thermal, mechanical and swelling properties of PVA/starch nanocomposite membranes incorporating gC 3 N 4 | |
CN109513039B (en) | Antibacterial hydrogel dressing containing imidazole bromide salt and preparation method and application thereof | |
CN107778497B (en) | Composite covalent hydrogel capable of releasing according to needs as well as preparation method and application thereof | |
CN106832347B (en) | A kind of safe and efficient durable antibiotic nano-hydrogel and preparation method thereof | |
Zhang et al. | Sodium alginate fasten cellulose nanocrystal Ag@ AgCl ternary nanocomposites for the synthesis of antibacterial hydrogels | |
CN108686252B (en) | Nano-silver antibacterial dressing with chitosan-poloxamer as matrix and preparation method and application thereof | |
CN112451738B (en) | Silver ion polysaccharide polymer antibacterial dressing and preparation method and application thereof | |
Yuan et al. | A cellulose/Konjac glucomannan–based macroporous antibacterial wound dressing with synergistic and complementary effects for accelerated wound healing | |
CN112851951B (en) | Dialdehyde chitosan grafted with epsilon-polylysine and preparation method and application thereof | |
CN114561046B (en) | Guanidine hyaluronic acid type antibacterial hydrogel and preparation method and application thereof | |
CN114392388A (en) | Hydrogel composition and application thereof | |
CN111166931A (en) | Methacrylic acid sericin/chitosan quaternary ammonium salt hydrogel and preparation method and application thereof | |
CN115105624B (en) | Marine polysaccharide-based efficient antibacterial film dressing and preparation method thereof | |
Karydis-Messinis et al. | Development, physicochemical characterization and in vitro evaluation of chitosan-fish gelatin-glycerol hydrogel membranes for wound treatment applications. | |
Jiang et al. | Preparation and study of cellulose-based ZnO NPs@ HEC/C-β-CD/Menthol hydrogel as wound dressing | |
Si et al. | A study of hybrid organic/inorganic hydrogel films based on in situ-generated TiO 2 nanoparticles and methacrylated gelatin | |
CN104857550A (en) | Polylysine-p-hydroxyphenylpropionic acid antibacterial hydrogel dressing and preparation method thereof | |
CN113663122B (en) | Anti-inflammatory, antibacterial and anti-tumor multifunctional hydrogel material and preparation method and application thereof | |
Estrada-Villegas et al. | UV-initiated crosslinking of electrospun chitosan/poly (ethylene oxide) nanofibers doped with ZnO-nanoparticles: Development of antibacterial nanofibrous hydrogel | |
CN104740141B (en) | A kind of antimicrobial spray and preparation method thereof | |
AU2021100755A4 (en) | Silver Nanocluster-based Chitosan Hydrogel Dressing and Its Preparation Method and Application |
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 |