CN113797391A - Coating for medical instrument and preparation method and application thereof - Google Patents
Coating for medical instrument and preparation method and application thereof Download PDFInfo
- Publication number
- CN113797391A CN113797391A CN202111134838.6A CN202111134838A CN113797391A CN 113797391 A CN113797391 A CN 113797391A CN 202111134838 A CN202111134838 A CN 202111134838A CN 113797391 A CN113797391 A CN 113797391A
- Authority
- CN
- China
- Prior art keywords
- coating
- zinc
- salt
- strontium
- substrate
- 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
- 239000011248 coating agent Substances 0.000 title claims abstract description 83
- 238000000576 coating method Methods 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 75
- 150000003751 zinc Chemical class 0.000 claims abstract description 24
- 150000008442 polyphenolic compounds Chemical class 0.000 claims abstract description 22
- 235000013824 polyphenols Nutrition 0.000 claims abstract description 21
- 159000000008 strontium salts Chemical class 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000007800 oxidant agent Substances 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 230000001590 oxidative effect Effects 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 19
- 239000004246 zinc acetate Substances 0.000 claims description 19
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 18
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 18
- 239000000919 ceramic Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 16
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 16
- 229910001631 strontium chloride Inorganic materials 0.000 claims description 14
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 claims description 14
- UBXAKNTVXQMEAG-UHFFFAOYSA-L strontium sulfate Chemical compound [Sr+2].[O-]S([O-])(=O)=O UBXAKNTVXQMEAG-UHFFFAOYSA-L 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 239000002953 phosphate buffered saline Substances 0.000 claims description 10
- WMBWREPUVVBILR-WIYYLYMNSA-N (-)-Epigallocatechin-3-o-gallate Chemical compound O([C@@H]1CC2=C(O)C=C(C=C2O[C@@H]1C=1C=C(O)C(O)=C(O)C=1)O)C(=O)C1=CC(O)=C(O)C(O)=C1 WMBWREPUVVBILR-WIYYLYMNSA-N 0.000 claims description 9
- WMBWREPUVVBILR-UHFFFAOYSA-N GCG Natural products C=1C(O)=C(O)C(O)=CC=1C1OC2=CC(O)=CC(O)=C2CC1OC(=O)C1=CC(O)=C(O)C(O)=C1 WMBWREPUVVBILR-UHFFFAOYSA-N 0.000 claims description 9
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 9
- 229940030275 epigallocatechin gallate Drugs 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 239000011592 zinc chloride Substances 0.000 claims description 9
- 235000005074 zinc chloride Nutrition 0.000 claims description 9
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 7
- 229960001763 zinc sulfate Drugs 0.000 claims description 7
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- XMOCLSLCDHWDHP-IUODEOHRSA-N epi-Gallocatechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@H]2O)=CC(O)=C(O)C(O)=C1 XMOCLSLCDHWDHP-IUODEOHRSA-N 0.000 claims description 6
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 6
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 6
- 239000007943 implant Substances 0.000 claims description 6
- 239000003973 paint Substances 0.000 claims description 6
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 6
- LOKCTEFSRHRXRJ-UHFFFAOYSA-I dipotassium trisodium dihydrogen phosphate hydrogen phosphate dichloride Chemical compound P(=O)(O)(O)[O-].[K+].P(=O)(O)([O-])[O-].[Na+].[Na+].[Cl-].[K+].[Cl-].[Na+] LOKCTEFSRHRXRJ-UHFFFAOYSA-I 0.000 claims description 5
- 230000000399 orthopedic effect Effects 0.000 claims description 5
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 claims description 4
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 3
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 3
- 239000001263 FEMA 3042 Substances 0.000 claims description 3
- XMOCLSLCDHWDHP-UHFFFAOYSA-N L-Epigallocatechin Natural products OC1CC2=C(O)C=C(O)C=C2OC1C1=CC(O)=C(O)C(O)=C1 XMOCLSLCDHWDHP-UHFFFAOYSA-N 0.000 claims description 3
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 3
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 3
- DZYNKLUGCOSVKS-UHFFFAOYSA-N epigallocatechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3cc(O)c(O)c(O)c3 DZYNKLUGCOSVKS-UHFFFAOYSA-N 0.000 claims description 3
- 229940074391 gallic acid Drugs 0.000 claims description 3
- 235000004515 gallic acid Nutrition 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 235000015523 tannic acid Nutrition 0.000 claims description 3
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 3
- 229940033123 tannic acid Drugs 0.000 claims description 3
- 229920002258 tannic acid Polymers 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 19
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 12
- 239000011247 coating layer Substances 0.000 abstract description 8
- 210000000988 bone and bone Anatomy 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000012620 biological material Substances 0.000 abstract description 3
- 230000003993 interaction Effects 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 description 58
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 54
- 229910052719 titanium Inorganic materials 0.000 description 54
- 239000004696 Poly ether ether ketone Substances 0.000 description 15
- 229920002530 polyetherether ketone Polymers 0.000 description 15
- 230000014509 gene expression Effects 0.000 description 14
- 238000002791 soaking Methods 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000002585 base Substances 0.000 description 11
- 210000004027 cell Anatomy 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000001963 growth medium Substances 0.000 description 9
- 230000011164 ossification Effects 0.000 description 8
- 238000004506 ultrasonic cleaning Methods 0.000 description 8
- 238000012258 culturing Methods 0.000 description 7
- 210000002901 mesenchymal stem cell Anatomy 0.000 description 7
- 102000002260 Alkaline Phosphatase Human genes 0.000 description 6
- 108020004774 Alkaline Phosphatase Proteins 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
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- 238000002386 leaching Methods 0.000 description 6
- 208000015181 infectious disease Diseases 0.000 description 5
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- 239000002253 acid Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000007853 buffer solution Substances 0.000 description 3
- 238000010609 cell counting kit-8 assay Methods 0.000 description 3
- 239000002861 polymer material Substances 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 238000007781 pre-processing Methods 0.000 description 3
- 238000003753 real-time PCR Methods 0.000 description 3
- 238000010839 reverse transcription Methods 0.000 description 3
- IZTQOLKUZKXIRV-YRVFCXMDSA-N sincalide Chemical compound C([C@@H](C(=O)N[C@@H](CCSC)C(=O)NCC(=O)N[C@@H](CC=1C2=CC=CC=C2NC=1)C(=O)N[C@@H](CCSC)C(=O)N[C@@H](CC(O)=O)C(=O)N[C@@H](CC=1C=CC=CC=1)C(N)=O)NC(=O)[C@@H](N)CC(O)=O)C1=CC=C(OS(O)(=O)=O)C=C1 IZTQOLKUZKXIRV-YRVFCXMDSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229910052712 strontium Inorganic materials 0.000 description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 3
- LSHVYAFMTMFKBA-TZIWHRDSSA-N (-)-epicatechin-3-O-gallate Chemical compound O([C@@H]1CC2=C(O)C=C(C=C2O[C@@H]1C=1C=C(O)C(O)=CC=1)O)C(=O)C1=CC(O)=C(O)C(O)=C1 LSHVYAFMTMFKBA-TZIWHRDSSA-N 0.000 description 2
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical group O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 2
- LSHVYAFMTMFKBA-UHFFFAOYSA-N ECG Natural products C=1C=C(O)C(O)=CC=1C1OC2=CC(O)=CC(O)=C2CC1OC(=O)C1=CC(O)=C(O)C(O)=C1 LSHVYAFMTMFKBA-UHFFFAOYSA-N 0.000 description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 2
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- 229910021645 metal ion Inorganic materials 0.000 description 1
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- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
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- PWYYWQHXAPXYMF-UHFFFAOYSA-N strontium(2+) Chemical compound [Sr+2] PWYYWQHXAPXYMF-UHFFFAOYSA-N 0.000 description 1
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Images
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/54—Biologically active materials, e.g. therapeutic substances
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
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- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/216—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials with other specific functional groups, e.g. aldehydes, ketones, phenols, quaternary phosphonium groups
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- Life Sciences & Earth Sciences (AREA)
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- Animal Behavior & Ethology (AREA)
- Oral & Maxillofacial Surgery (AREA)
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- Materials For Medical Uses (AREA)
Abstract
The invention belongs to the technical field of biological materials, and particularly relates to a coating for medical instruments, and a preparation method and application thereof. The coating comprises the following components: metal salt, polyphenol and oxidant, wherein the metal salt is selected from zinc salt and strontium salt. The medical device comprises a substrate and a coating layer on the surface of the substrate, wherein the coating layer is formed by the coating. The coating is applied to medical instruments through the interaction of zinc salt, strontium salt, polyphenol and an oxidant, and has the advantages of uniform film formation, no influence on the biocompatibility of a base material, improvement on the antibacterial property, promotion of bone effect, wide application range, simple and convenient preparation process, good repeatability, strong controllability and the like.
Description
Technical Field
The invention belongs to the technical field of biological materials, and particularly relates to a coating for medical instruments, and a preparation method and application thereof.
Background
In recent years, biomaterials have been used to build medical devices or implants to replace diseased or lost biological outcomes. The bio-inert surface of the orthopedic implant is the biggest obstacle to the application of biomedicine, and although implant materials such as metal, ceramic, high polymer materials and the like are widely used in orthopedic surgery, the problems of infection risk, poor osteogenesis and the like still exist. In the prior art, antibiotics, antibacterial metal ions, hydroxyapatite and the like are used as common solutions for solving the problems of infection and bone formation, but the problems of infection and bone formation are difficult to solve simultaneously and the method is complex.
Therefore, there is a need to develop a new medical device to effectively solve the problems of infection risk and poor osteogenesis.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides a coating for a medical device, and a preparation method and application thereof, so as to solve the problems of infection risk and poor osteogenesis of the existing medical device.
In a first aspect of the present invention, there is provided a paint, wherein the raw material components for preparing the paint comprise: metal salt, polyphenol, oxidant, wherein, the metal salt includes zinc salt and strontium salt.
Among them, zinc ions stimulate the formation and mineralization of bones, playing an important role in the formation process of bones. Strontium, a physiological trace element, inhibits the generation of osteoclasts, accumulates in bones, promotes the proliferation and differentiation of mesenchymal stem cells or osteoblasts, accelerates the formation of new bones, is an important regulator of bone resorption, and can also induce the apoptosis of osteoclasts. Has been used as one of the drugs for treating osteoporosis. Polyphenols, widely distributed in plant tissues, are associated with a variety of biological functions, such as chemical defense, pigmentation, structural support and protection against radiation damage; has strong solid-liquid interface activity.
According to some embodiments of the invention, the zinc salt is at least one of zinc acetate, zinc chloride, zinc sulfate, zinc nitrate.
According to some embodiments of the invention, the zinc salt is zinc acetate. According to some embodiments of the invention, the zinc salt is zinc chloride. According to some embodiments of the invention, the zinc salt is zinc sulfate. According to some embodiments of the invention, the zinc salt is zinc nitrate. According to some embodiments of the invention, the zinc salt is zinc acetate, zinc chloride, zinc sulfate, and zinc nitrate. According to some embodiments of the invention, the zinc salt is zinc acetate, zinc chloride and zinc sulfate. According to some embodiments of the invention, the zinc salt is zinc chloride, zinc sulfate, or zinc nitrate. According to some embodiments of the invention, the zinc salt is zinc acetate, zinc chloride, and zinc nitrate. According to some embodiments of the invention, the zinc salt is zinc chloride or zinc nitrate. According to some embodiments of the invention, the zinc salt is zinc acetate or zinc chloride. According to some embodiments of the invention, the zinc salt is zinc acetate and zinc sulfate. According to some embodiments of the invention, the zinc salt is zinc acetate or zinc nitrate.
According to some embodiments of the invention, the strontium salt is at least one of strontium chloride, strontium sulfate, strontium carbonate.
According to some embodiments of the invention, the strontium salt is strontium chloride. According to some embodiments of the invention, the strontium salt is strontium sulfate. According to some embodiments of the invention, the strontium salt is strontium carbonate. According to some embodiments of the invention, the strontium salt is strontium chloride and strontium sulfate. According to some embodiments of the invention, the strontium salt is strontium chloride or strontium carbonate. According to some embodiments of the invention, the strontium salt is strontium sulfate and strontium carbonate. According to some embodiments of the invention, the strontium salt is strontium chloride, strontium sulfate and strontium carbonate.
According to some embodiments of the invention, the polyphenol is at least one of epigallocatechin gallate, epicatechin gallate, epigallocatechin, tannic acid, dopamine hydrochloride, gallic acid, pyrogallol.
According to some embodiments of the invention, the polyphenol is epigallocatechin gallate. According to some embodiments of the invention, the polyphenol is epicatechin gallate. According to some embodiments of the invention, the polyphenol is epigallocatechin. According to some embodiments of the invention, the polyphenol is tannic acid. According to some embodiments of the invention, the polyphenol is dopamine hydrochloride. According to some embodiments of the invention, the polyphenol is gallic acid. According to some embodiments of the invention, the polyphenol is pyrogallic acid.
According to some embodiments of the invention, the oxidizing agent is at least one of hydrogen peroxide, ammonium persulfate.
According to some embodiments of the invention, the oxidizing agent is hydrogen peroxide. According to some embodiments of the invention, the oxidant is ammonium persulfate.
According to some embodiments of the invention, the molar concentration of the zinc salt is 0.001 to 5 mol/L. According to some embodiments of the invention, the molar concentration of the zinc salt is from 0.001 to 1 mol/L.
According to some embodiments of the invention, the zinc salt is zinc acetate, and the mass concentration of the zinc acetate is 7.339-36696 mg/L. According to some embodiments of the invention, the zinc salt is zinc acetate, and the mass concentration of the zinc acetate is 7.339-7339 mg/L. According to some embodiments of the invention, the strontium salt is present in a molar concentration of 0.001-5 mol/L. According to some embodiments of the invention, the strontium salt is present in a molar concentration of 0.001-1 mol/L.
According to some embodiments of the invention, the strontium salt is strontium chloride, and the mass concentration of the strontium chloride is 6.341-31706 mg/L.
According to some embodiments of the invention, the mass concentration of the polyphenol is 0.1 to 5 g/L. According to some embodiments of the invention, the mass concentration of the polyphenol is 0.1 to 1 g/L.
According to some embodiments of the invention, the oxidant is 0.01-1% by mass.
According to some embodiments of the invention, the feedstock component further comprises a solvent.
According to some embodiments of the invention, the solvent has a pH of 7 to 10. According to some embodiments of the invention, the solvent has a pH of 7.5 to 9.5.
According to some embodiments of the invention, the solvent is at least one of a phosphate buffered saline solution, a tris hydrochloride solution.
According to some embodiments of the invention, the solvent is a phosphate buffered saline solution. According to some embodiments of the invention, the solvent is tris hydrochloride solution. According to some embodiments of the invention, the solvent is a phosphate buffered saline solution and a tris hydrochloride solution.
In a second aspect of the present invention, a method for preparing the above coating is provided, which comprises the following steps: and mixing the raw material components to obtain the coating.
According to some embodiments of the invention, the mixing temperature is 50-120 ℃ and the mixing time is 0.5-24 h.
According to some embodiments of the invention, the mixing temperature is 70-90 ℃ and the mixing time is 2-10 h.
According to some embodiments of the invention, the mixing temperature is 80 ℃ and the mixing time is 3-8 h.
In a third aspect of the invention, a medical device is provided, which comprises a substrate and a coating layer on the surface of the substrate, wherein the coating layer is formed by the coating material.
According to some embodiments of the invention, the substrate is at least one of a metal, a ceramic, a polymer material.
According to some embodiments of the invention, the substrate is a metal. According to some embodiments of the invention, the substrate is a titanium substrate.
According to some embodiments of the invention, the substrate is ceramic. According to some embodiments of the invention, the substrate is a medical ceramic sheet.
According to some embodiments of the invention, the substrate is a polymeric material. According to some embodiments of the invention, the substrate is polyetheretherketone.
According to some embodiments of the invention, the ratio of the volume of the coating (in milliliters) to the surface area of the substrate (in square centimeters) is from 0.01 to 0.2.
According to some embodiments of the invention, the medical device is an orthopedic implant.
In a fourth aspect of the present invention, there is provided a method for preparing the above medical device, comprising the steps of:
(1) pretreating the base material to obtain a pretreated base material;
(2) and placing the pretreated substrate in the coating for reaction to obtain the medical instrument.
In the reaction, polyphenol, metal salt and oxidant interact, the benzene hydroxyl of polyphenol reacts with oxidant to become benzoquinone group, and the benzoquinone group is chelated with zinc ion and strontium ion to form stable coating on the surface of the pretreated base material.
According to some embodiments of the invention, the pre-processing step comprises: soaking the substrate in plasma, acid or alkali. In the soaking process, a large number of active groups are attached to the surface of the substrate, so that the substrate and polyphenol form a firm coating in a short reaction time.
According to some embodiments of the invention, the pre-processing step comprises: and carrying out ultrasonic cleaning on the substrate, and then soaking the substrate in plasma, acid or alkali for activation.
According to some embodiments of the invention, the base is sodium hydroxide solution. According to some embodiments of the invention, the concentration of the base is 1 to 10 mol/L.
According to some embodiments of the invention, the temperature of the soaking is 40-100 ℃. According to some embodiments of the invention, the temperature of the soaking is 55-80 ℃.
According to some embodiments of the invention, the soaking time is 4-10 h. According to some embodiments of the invention, the soaking time is 5-8 h.
According to some embodiments of the invention, the solvent for the ultrasonic cleaning is at least one of acetone, ethanol, and deionized water.
According to some embodiments of the invention, the step of ultrasonically cleaning comprises: sequentially placing in acetone, ethanol, and deionized water, and ultrasonic cleaning for 10-20 min.
According to some embodiments of the invention, the pre-processing step comprises: and (3) grinding and polishing the substrate, ultrasonically cleaning the substrate, and then soaking the substrate in plasma, acid or alkali for activation. According to some embodiments of the present invention, 400-2000 mesh sandpaper is used for sanding and polishing.
According to some embodiments of the invention, the soaking step is followed by a rinsing step. According to some embodiments of the invention, the cleaning is ultrasonic cleaning in deionized water for 10-25 min.
According to some embodiments of the invention, the reaction is a hydrothermal reaction. According to some embodiments of the invention, the temperature of the reaction is 50 to 120 ℃ and the time of the reaction is 0.5 to 24 hours.
According to some embodiments of the invention, the reaction is followed by a washing and drying step. According to some embodiments of the invention, the rinsing is performed with deionized water and the drying is performed in a vacuum drying manner.
In a fifth aspect of the invention, there is provided the use of a coating as described above in the manufacture of a medical device.
According to some embodiments of the invention, the medical device is an orthopedic implant.
Compared with the prior art, the invention has the following beneficial effects:
(1) the coating disclosed by the invention takes zinc salt, strontium salt, polyphenol and an oxidant as raw material components, and a coating is formed on the surface of a base material through the interaction of the zinc salt, the strontium salt, the polyphenol and the oxidant, so that the film is formed uniformly, and the biocompatibility of the base material is not influenced;
(2) the coating disclosed by the invention is applied to medical instruments, and can improve the antibacterial property of the medical instruments;
(3) the coating disclosed by the invention is applied to medical instruments, has a good effect of promoting bone formation, and provides important research value and clinical significance for a bone grafting technology.
(4) The coating has wide application range and comprises metal, ceramic and high polymer materials.
(5) The coating provided by the invention is simple and convenient in preparation process, good in repeatability and strong in controllability.
Drawings
FIG. 1 is a surface topography of a titanium substrate according to example 1 of the present invention;
FIG. 2 shows the results of the cytocompatibility test of the titanium substrate of example 1;
FIG. 3 shows the results of the bone-promoting effect test of the titanium substrate of example 1;
fig. 4 shows the antibacterial property test results of the titanium substrate of example 1 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.
Example 1
A titanium substrate coated with a coating layer, comprising a 1X 2cm titanium substrate and a coating layer formed on the surface of the titanium substrate by a paint. The raw material components for preparing the coating comprise: 40mg of epigallocatechin gallate, 20mg of zinc acetate, 41mg of strontium chloride, 20mg of ammonium persulfate, and 40mL of a phosphate buffered saline (i.e., PBS buffer, pH 8.0).
The preparation method of the titanium substrate coated by the coating comprises the following steps:
(1) sequentially and respectively placing the titanium substrate in acetone, ethanol and deionized water for ultrasonic cleaning for 15min to obtain a cleaned titanium substrate;
(2) soaking the cleaned titanium substrate in a sodium hydroxide solution (the molar concentration is 4mol/L) at 60 ℃ for 8 hours to obtain a soaked titanium substrate;
(3) placing the soaked titanium substrate in deionized water, ultrasonically cleaning for 20min, and drying to obtain a pretreated titanium substrate;
(4) mixing epigallocatechin gallate, zinc acetate, strontium chloride, ammonium persulfate and PBS buffer solution (pH value is 8.0), and stirring to obtain coating;
(5) and (3) placing the pretreated titanium substrate and the coating into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 5 hours at 80 ℃, then placing into deionized water, ultrasonically cleaning, and drying to obtain the titanium substrate coated with the coating.
Example 2
A coating-coated polyetheretherketone comprises polyetheretherketone and a coating layer formed by a coating on the surface of the polyetheretherketone. The polyetheretherketone is a cylinder with a diameter of 1cm and a height of 3 cm.
The raw material components for preparing the coating comprise: 20mg of epigallocatechin gallate, 30mg of zinc acetate, 30mg of strontium chloride, 30mg of ammonium persulfate and 40mL of Tris-HCl buffer solution (pH 7.5).
The preparation method of the polyether-ether-ketone coated by the coating comprises the following steps:
(1) sequentially and respectively placing polyether-ether-ketone in acetone, ethanol and deionized water for ultrasonic cleaning for 10min to obtain cleaned polyether-ether-ketone;
(2) soaking the cleaned polyether-ether-ketone in a sodium hydroxide solution (the molar concentration is 3mol/L) at 60 ℃ for 5 hours to obtain soaked polyether-ether-ketone;
(3) placing the soaked polyether-ether-ketone in deionized water, ultrasonically cleaning for 10min, and drying to obtain pretreated polyether-ether-ketone;
(4) mixing epigallocatechin gallate, zinc acetate, strontium chloride, ammonium persulfate and tris (hydroxymethyl) aminomethane hydrochloride solution, and stirring uniformly to obtain a coating;
(5) and (3) placing the pretreated polyether-ether-ketone and the coating into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, and reacting for 2 hours at 80 ℃ to obtain the polyether-ether-ketone coated by the coating.
Example 3
A medical ceramic piece coated by a coating comprises a medical ceramic piece with the thickness of 1 x 3cm and a coating formed by paint on the surface of the medical ceramic piece.
The raw material components for preparing the coating comprise: 40mg of epigallocatechin gallate, 30mg of zinc acetate, 30mg of strontium chloride, 40mg of ammonium persulfate and 40mL of Tris-HCl buffer solution (pH 7.5).
The preparation method of the medical ceramic sheet coated by the coating comprises the following steps:
(1) sequentially and respectively placing the medical ceramic wafer in acetone, ethanol and deionized water for ultrasonic cleaning for 10min to obtain a cleaned medical ceramic wafer;
(2) soaking the cleaned medical ceramic wafer in a sodium hydroxide solution (the molar concentration is 3mol/L) at 70 ℃ for 6 hours to obtain a soaked medical ceramic wafer;
(3) placing the soaked medical ceramic wafer in deionized water for ultrasonic cleaning for 10min, and drying to obtain pretreated polyether-ether-ketone;
(4) mixing epigallocatechin gallate, zinc acetate, strontium chloride, ammonium persulfate and tris (hydroxymethyl) aminomethane hydrochloride solution, and stirring uniformly to obtain a coating;
(5) and (3) placing the pretreated medical ceramic sheet and the coating into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, and reacting for 3 hours at 80 ℃ to obtain the medical ceramic sheet coated with the coating.
Product performance detection
1. Surface topography analysis
Scanning electron microscope surface morphology scanning and energy spectrometer element analysis are carried out on the titanium base material before and after the coating of the embodiment 1, and a surface morphology diagram of the titanium base material of the embodiment 1 of the invention shown in figure 1 and an element analysis result of the surface of the titanium base material after the coating is coated shown in table 1 are obtained.
In fig. 1, a is a surface topography of the titanium substrate before being coated with the coating in example 1 of the present invention, and B is a surface topography of the titanium substrate after being coated with the coating in example 1 of the present invention. According to the figure 1, the surface of the titanium substrate coated by the coating is uniformly formed.
According to table 1, the average mass percent of zinc and the average mass percent of strontium on the surface of the titanium substrate after coating in example 1 of the present invention were 7.687% and 2.421%, respectively.
TABLE 1 elemental analysis Table for the surface of titanium substrate coated with the coating layer in inventive example 1
| Mass percent | Zinc (wt%) | Strontium (wt%) |
| 1 | 7.680 | 2.016 |
| 2 | 8.228 | 3.144 |
| 3 | 7.152 | 2.104 |
2. Cell compatibility test
Respectively placing the titanium substrate before coating of the embodiment 1 and the titanium substrate after coating of the embodiment 1 in a fresh culture medium for soaking for 24 hours, obtaining leaching liquor of the titanium substrate and sterilizing the leaching liquor to obtain leaching liquor A and leaching liquor B;
5X 10 per well in 96-well plates4Culturing an L929 cell plate at 37 ℃ for 24 hours, removing a culture medium, adding leaching liquor A, culturing at 37 ℃ for 24 hours, removing the culture medium, washing with PBS for 3 times, adding 100uL of CCK-8, incubating at 37 ℃ for 1 hour, measuring the light absorption value with the wavelength of 450nm, and calculating relative activity to obtain the cell activity level of the titanium substrate before coating in the embodiment 1 of the invention;
5X 10 per well in 96-well plates4Culturing an L929 cell plate at 37 ℃ for 24 hours, removing a culture medium, adding leaching liquor B, culturing at 37 ℃ for 24 hours, removing the culture medium, washing with PBS for 3 times, adding 100uL of CCK-8, incubating at 37 ℃ for 1 hour, measuring the light absorption value with the wavelength of 450nm, and calculating relative activity to obtain the cell activity level of the titanium substrate coated by the coating in the embodiment 1 of the invention;
5X 10 per well in 96-well plates4Culturing the L929 cell plates at 37 ℃ for 24h, removing the culture medium, culturing at 37 ℃ for 24h, removing the culture medium, washing with PBS for 3 times, adding 100uL of CCK-8, incubating at 37 ℃ for 1h, measuring the absorbance value at the wavelength of 450nm, and calculating the relative activity to obtain the cell activity level of a control group.
FIG. 2 is the result of the cytocompatibility test of the titanium substrate of example 1, wherein the ordinate "cell Viability" is the cell activity, the bar corresponding to "control" on the abscissa is the cell activity level of the control group, and the bar corresponding to "Ti" is the cell activity level of the titanium substrate before being coated with the coating of example 1; the bar corresponding to "modified Ti" is the level of cellular activity of the titanium substrate coated with the coating of example 1 of the present invention.
According to FIG. 2, the level of cellular activity was 100% before and after coating. Therefore, coating does not affect the cell compatibility of the titanium substrate.
(3) Test for bone-promoting effect
Respectively sterilizing the titanium substrate before coating and the titanium substrate after coating in the embodiment 1 of the invention;
in 6-well plates, 1X 10 wells per well6A plate of MSCs (mesenchymal Stem cells) was added to the plate of the present invention in example 1Culturing the titanium substrate before coating for 24h at 37 ℃, removing the culture medium, extracting RNA, performing reverse transcription, and measuring the gene expression level of alkaline phosphatase (ALP) by qPCR (real-time fluorescent quantitative PCR method) to obtain the gene expression level of the titanium substrate before coating in the embodiment 1 of the invention;
in 6-well plates, 1X 10 wells per well6Adding the coating-coated titanium substrate of the embodiment 1 of the invention into a MSCs (mesenchymal stem cell) plate, culturing at 37 ℃ for 24h, removing the culture medium, extracting RNA, performing reverse transcription, and measuring the gene expression level of alkaline phosphatase (ALP) by qPCR (real-time fluorescent quantitative PCR) to obtain the gene expression level of the coating-coated titanium substrate of the embodiment 1 of the invention;
in 6-well plates, 1X 10 wells per well6Each MSCs (mesenchymal stem cell) plate was cultured at 37 ℃ for 24 hours, the medium was removed, RNA was extracted, reverse transcription was performed, and the gene expression level of alkaline phosphatase (ALP) was measured by qPCR (i.e., real-time fluorescent quantitative PCR method) to obtain the gene expression level of the control group.
FIG. 3 is a result of bone-promoting effect test of the titanium substrate according to example 1 of the present invention, in which the ordinate "Relative mRNA Expression" indicates the gene Expression level, the bar corresponding to "control" on the abscissa indicates the gene Expression level of the control group, the bar corresponding to "Ti" on the abscissa indicates the gene Expression level of the titanium substrate before coating, and the bar corresponding to "modified Ti" on the abscissa indicates the gene Expression level of the titanium substrate after coating. Referring to FIG. 3, the gene expression level of the titanium substrate before coating of example 1 of the present invention was lower than that of the control group, indicating that it contributes to poor bone effect; the gene expression level of the titanium substrate coated by the coating of the embodiment 1 is far greater than that of the control group, which shows that the gene expression level is good in bone formation promoting effect, so that the coating provided by the embodiment 1 can improve the bone formation effect of the titanium substrate.
(3) Antibacterial property test
The titanium substrate before coating and the titanium substrate after coating of example 1 of the present invention were immersed in bacterial suspensions (1X 10)8CFU/mL), cultured in a constant temperature shaking incubator for 4h (37 ℃, 200 rpm). Warp beamAfter the culture, an appropriate amount of the diluted bacterial suspension was applied to an agar medium and cultured at 37 ℃ for 12 hours. The antibacterial ratio was calculated by counting the number of colonies, and the antibacterial test result of the titanium substrate of example 1 of the present invention shown in fig. 4 was obtained. Wherein, A1 and A2 correspond to the antibacterial property test results of the titanium base material before being coated by the coating of the embodiment 1 of the invention; b1 and B2 correspond to the antibacterial property test results of the titanium substrate coated by the coating of the embodiment 1 of the invention.
According to fig. 4, the antibacterial property of the titanium substrate before being coated with the coating of example 1 is poor, and the antibacterial property of the titanium substrate after being coated with the coating of example 1 is improved, so that the antibacterial property of the titanium substrate can be improved by the coating prepared by the invention.
The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The paint is characterized in that raw material components for preparing the paint comprise: metal salt, polyphenol, oxidant, wherein, the metal salt includes zinc salt and strontium salt.
2. The coating of claim 1, wherein the zinc salt is at least one of zinc acetate, zinc chloride, zinc sulfate, zinc nitrate; the strontium salt is at least one of strontium chloride, strontium sulfate and strontium carbonate; the polyphenol is at least one of epigallocatechin gallate, epigallocatechin, tannic acid, dopamine hydrochloride, gallic acid and pyrogallic acid; the oxidant is at least one of hydrogen peroxide and ammonium persulfate.
3. The coating according to claim 1, characterized in that the molar concentration of the zinc salt is 0.001-5 mol/L; the molar concentration of the strontium salt is 0.001-5 mol/L; the mass concentration of the polyphenol is 0.1-5 g/L; the mass percentage of the oxidant is 0.01-1%.
4. The coating of claim 1, wherein the feedstock components further comprise a solvent comprising at least one of a phosphate buffered saline solution, a tris hydrochloride solution.
5. A method for preparing a coating according to any one of claims 1 to 4, characterized in that it comprises the following steps:
and mixing the raw material components to obtain the coating.
6. A medical device comprising a substrate and a coating on a surface of the substrate, the coating being formed from the coating of any one of claims 1 to 4.
7. The medical device of claim 6, wherein the substrate is at least one of a metal, a ceramic, and a polymeric material.
8. The medical device of claim 6, wherein the medical device is an orthopedic implant.
9. A method of manufacturing a medical device according to any of claims 6 to 8, comprising the steps of:
pretreating the base material to obtain a pretreated base material;
and placing the pretreated substrate in the coating for reaction to obtain the medical instrument.
10. Use of a coating according to any one of claims 1 to 4 in the manufacture of a medical device.
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