CN111494218B - Bioactive glass - Google Patents
Bioactive glass Download PDFInfo
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- CN111494218B CN111494218B CN202010036388.6A CN202010036388A CN111494218B CN 111494218 B CN111494218 B CN 111494218B CN 202010036388 A CN202010036388 A CN 202010036388A CN 111494218 B CN111494218 B CN 111494218B
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- bioactive glass
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- tooth structure
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- 239000005313 bioactive glass Substances 0.000 title claims abstract description 132
- 239000011521 glass Substances 0.000 claims abstract description 27
- 229910001634 calcium fluoride Inorganic materials 0.000 claims abstract description 5
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims abstract description 5
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 60
- 239000000203 mixture Substances 0.000 claims description 33
- 239000002245 particle Substances 0.000 claims description 19
- 210000005239 tubule Anatomy 0.000 claims description 18
- 208000002925 dental caries Diseases 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 239000006060 molten glass Substances 0.000 claims description 12
- 206010020751 Hypersensitivity Diseases 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 10
- 229910018068 Li 2 O Inorganic materials 0.000 claims description 10
- 230000000395 remineralizing effect Effects 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 208000026935 allergic disease Diseases 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 210000003298 dental enamel Anatomy 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- 230000009610 hypersensitivity Effects 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- 239000000499 gel Substances 0.000 claims description 6
- 238000010791 quenching Methods 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 230000003239 periodontal effect Effects 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 4
- 210000003074 dental pulp Anatomy 0.000 claims description 4
- DLYUQMMRRRQYAE-UHFFFAOYSA-N phosphorus pentoxide Inorganic materials O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000000606 toothpaste Substances 0.000 claims description 4
- 208000006558 Dental Calculus Diseases 0.000 claims description 3
- 239000000839 emulsion Substances 0.000 claims description 3
- 239000006210 lotion Substances 0.000 claims description 3
- 239000002324 mouth wash Substances 0.000 claims description 3
- 239000002674 ointment Substances 0.000 claims description 3
- 239000006072 paste Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 230000008439 repair process Effects 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000001356 surgical procedure Methods 0.000 claims description 3
- 235000015218 chewing gum Nutrition 0.000 claims description 2
- 239000000551 dentifrice Substances 0.000 claims description 2
- 239000003937 drug carrier Substances 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 229940034610 toothpaste Drugs 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims 3
- 229910052906 cristobalite Inorganic materials 0.000 claims 3
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims 3
- 229910052682 stishovite Inorganic materials 0.000 claims 3
- 229910052905 tridymite Inorganic materials 0.000 claims 3
- 239000003242 anti bacterial agent Substances 0.000 claims 1
- 229940112822 chewing gum Drugs 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229940051866 mouthwash Drugs 0.000 claims 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 abstract description 32
- 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 abstract description 32
- 239000000463 material Substances 0.000 abstract description 5
- 230000004071 biological effect Effects 0.000 abstract description 4
- 230000033558 biomineral tissue development Effects 0.000 abstract description 4
- 239000006121 base glass Substances 0.000 abstract description 2
- 229910001947 lithium oxide Inorganic materials 0.000 abstract description 2
- 239000012890 simulated body fluid Substances 0.000 description 21
- 230000000694 effects Effects 0.000 description 18
- 210000004268 dentin Anatomy 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 238000002441 X-ray diffraction Methods 0.000 description 12
- 238000002425 crystallisation Methods 0.000 description 12
- 230000008025 crystallization Effects 0.000 description 12
- 239000000126 substance Substances 0.000 description 11
- 230000009286 beneficial effect Effects 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 210000000988 bone and bone Anatomy 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 7
- 229910052593 corundum Inorganic materials 0.000 description 7
- 239000010431 corundum Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 6
- 230000003266 anti-allergic effect Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000009472 formulation Methods 0.000 description 5
- 239000000395 magnesium oxide Substances 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 4
- 239000005312 bioglass Substances 0.000 description 4
- 230000001680 brushing effect Effects 0.000 description 4
- 201000002170 dentin sensitivity Diseases 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 210000001519 tissue Anatomy 0.000 description 4
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 3
- 239000010839 body fluid Substances 0.000 description 3
- 210000001124 body fluid Anatomy 0.000 description 3
- 229910001424 calcium ion Inorganic materials 0.000 description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 239000008213 purified water Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- 239000004599 antimicrobial Substances 0.000 description 2
- 229910052586 apatite Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000000975 bioactive effect Effects 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000001506 calcium phosphate Substances 0.000 description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 description 2
- 235000011010 calcium phosphates Nutrition 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000003203 everyday effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000007496 glass forming Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 210000000214 mouth Anatomy 0.000 description 2
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[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 VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 2
- 208000028169 periodontal disease Diseases 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 208000024891 symptom Diseases 0.000 description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 206010061363 Skeletal injury Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 210000000845 cartilage Anatomy 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 210000002808 connective tissue Anatomy 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004031 devitrification Methods 0.000 description 1
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000004962 physiological condition Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000002980 postoperative effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 210000004872 soft tissue Anatomy 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 230000036347 tooth sensitivity Effects 0.000 description 1
- 230000029663 wound healing Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/02—Inorganic compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/20—Halogens; Compounds thereof
- A61K8/21—Fluorides; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/24—Phosphorous; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/25—Silicon; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/025—Other specific inorganic materials not covered by A61L27/04 - A61L27/12
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/10—Ceramics or glasses
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/12—Phosphorus-containing materials, e.g. apatite
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- 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
- A61L27/60—Materials for use in artificial skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/04—Materials or treatment for tissue regeneration for mammary reconstruction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/06—Materials or treatment for tissue regeneration for cartilage reconstruction, e.g. meniscus
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/34—Materials or treatment for tissue regeneration for soft tissue reconstruction
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Epidemiology (AREA)
- Inorganic Chemistry (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Medicinal Chemistry (AREA)
- Birds (AREA)
- Dermatology (AREA)
- Transplantation (AREA)
- Pharmacology & Pharmacy (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Glass Compositions (AREA)
- Cosmetics (AREA)
Abstract
The invention relates to bioactive glass, and belongs to the field of materials. Compared with the base glass, the glass provided by the invention also contains a certain amount of lithium oxide and calcium fluoride, has a high mineralization rate, can quickly form hydroxyapatite, has good biological activity, and can be used for teeth and the like.
Description
Technical Field
The invention relates to bioactive glass, and belongs to the field of materials.
Background
Bioactive glass was developed by Hench professor of florida university in the united states in 1969, and besides the 45S5 bioactive glass formulation developed by Hench professor, various bioactive glasses have been continuously developed, and although these new bioactive glasses improve mechanical properties, biocompatibility and the like to some extent, the 45S5 bioactive glass formulation is still a well-recognized formulation with better bioactivity.
The bioactive glass is a glass with a special composition structure, and the special composition and structure endow the bioactive glass with good bioactivity, and can be used as a bioactive material for repairing teeth, bones, skin and the like of a human body. Bioactive glass bioactivity is the result of a complex series of physiochemical reactions on the surface of glass under physiological conditions. When the bioactive glass is applied to human body, the bioactive glass can perform close ion exchange with human body liquid, and finally form a hydroxyapatite layer similar to teeth, bones, skin and other components. Currently, bioactive glass has been successfully applied to the fields of treatment and repair of bone injuries, periodontal defects and the like. In recent years, the treatment of tooth sensitivity using bioactive glass containing calcium, phosphorus and silicon components has become a research hotspot. The bioactive glass is smeared on the exposed dentin tubule, an apatite layer is gradually adhered on the dentin tubule, and apatite crystals are formed in the tubule, so that the exposed dentin tubule is sealed, and dentin hypersensitivity is effectively improved.
Although 45S5 bioactive glass has a certain mineralization antiallergic effect, the required mineralization time is longer, namely the onset of action is slower, and the problem of dentin hypersensitivity cannot be rapidly and effectively solved. Therefore, there is a need for further improvements in the bioactivity of bioactive glasses which are expected to achieve rapid and sustained results and which are able to prevent, alleviate and/or radically treat a variety of conditions including dental hypersensitivity.
Disclosure of Invention
The invention provides bioactive glass with better bioactivity on the basis of 45S5 bioactive glass. When the bioactive glass provided by the invention is applied, hydroxyapatite can be rapidly formed, the bioactive glass can be used for rapidly closing dentinal tubules in the aspect of oral cavity and teeth, and has remarkable anti-sensitivity effect in preventing, relieving and/or radically curing dental hypersensitive symptoms, and simultaneously has the functions of preventing dental caries, repairing damaged enamel and the like.
When placed in a Simulated Body Fluid (SBF), the bioactive glass of the present invention can form a Hydroxyapatite (HCA) layer in vitro. The formation of hydroxyapatite begins with the bioactive glass contacting the simulated body fluid. In the context of the present invention, a bioactive glass is considered bioactive if it is exposed to Simulated Body Fluid (SBF) to form a crystallized layer of HCA within 24 hours.
The bioactive glass provided by the invention comprises the following components in terms of oxide mass (wt.%):
The bioactive glass provided by the invention contains Li 2 O (lithium oxide), and the radius of lithium ions is much smaller than that of sodium ions, so that the glass structure is more loose due to the addition of lithium ions; in the invention, the Li 2 O accounting for 0.5 to 2.5 percent of the oxide mass is added to loosen the glass structure, the glass network is easy to disintegrate, the glass activity is larger, the glass forming performance of the glass is not influenced, and the antiallergic speed and effect of the active glass are improved.
The bioactive glass provided by the invention contains a proper amount of CaF 2 (calcium fluoride), the proper amount is 2.0% -9.0% (based on the amount of oxidized substances), and the proper amount of CaF 2 is beneficial to improving the speed of forming hydroxyapatite by the bioactive glass in human body fluid environment and improving the antiallergic speed and effect of the bioactive glass.
The proper amount of CaF 2 and the proper amount of Li 2 O are beneficial to improving the speed of forming the hydroxyapatite by the bioactive glass in the human body fluid environment, and can also give consideration to the glass forming performance. The inventor finds that the activity of the bioactive glass is remarkably improved when the mass ratio of the Li 2 O to the CaF 2 is 0.11-0.16, and the CaF 2 is 5.55-7.66%, the Li 2 O is 0.84-1.25% and the mass ratio of the Li 2 O to the CaF 2 in the bioactive glass is calculated according to the oxidation mass.
The addition of barium element to the glass can cause a part of Ca 2+ in the generated hydroxyapatite to be replaced, thus generating mixed Ba 2+/Ca2+ hydroxyapatite, and the generated hydroxyapatite has increased deposition rate due to the lower solubility of the Ba 2+ substituted hydroxyapatite than the unsubstituted hydroxyapatite, thus showing stronger activity of the glass. The bioactive glass provided by the invention contains a proper amount of BaO (barium oxide), the proper amount is 1.0% -3.0% (based on the amount of oxidized substances), and the proper amount of BaO is beneficial to improving the speed of forming hydroxyapatite in the human body fluid environment of the bioactive glass and improving the acid corrosion resistance of the glass, so that the antiallergic speed of the bioactive glass is improved and the effect is more durable.
The magnesium element exists in the glass as a network modifier, and the addition of the magnesium element to the glass can distort the structure of the glass and destroy the original structure of the bioactive glass, so that the glass has a faster ion release rate and the activity is improved. The bioactive glass provided by the invention contains a proper amount of MgO (magnesium oxide), wherein the proper amount is 1.0% -3.0% (based on the amount of oxidized substances), and the proper amount of MgO is beneficial to improving the acid corrosion resistance of the bioactive glass, so that the antiallergic speed of the bioactive glass is beneficial to being improved, and the effect is more durable.
The bioactive glass provided by the invention further comprises SiO 2 (silicon dioxide), P 2O5 (phosphorus pentoxide), na 2 O (sodium oxide) and CaO (calcium oxide) according to the amount of oxide substances.
SiO 2 forms an amorphous network of bioactive glass and the percentage of SiO 2 affects its network connectivity. The bioactive glass provided by the invention contains SiO 2 35.0.0% -40.0% according to the amount of oxide substances, and is beneficial to improving the activity of the bioactive glass by matching with other components.
The surface of the bioactive glass releases phosphate ions that contribute to the formation of hydroxyapatite. Although hydroxyapatite may be formed without the bioactive glass providing phosphate ions, the bioactive glass providing phosphate ions may increase the rate of formation of hydroxyapatite. The bioactive glass provided by the invention contains P 2O5 8.0.0% -11.0% according to the amount of oxide substances, and is beneficial to improving the activity of the bioactive glass by matching with other components.
The release of calcium ions from the surface of the bioactive glass aids in the formation of a calcium phosphate-rich layer on the surface of the glass. The bioactive glass provides calcium ions to increase the rate of formation of the calcium phosphate-rich layer. The bioactive glass provided by the invention contains 18.0% -22.0% of CaO according to the amount of oxide substances, and is beneficial to improving the activity of the bioactive glass by matching with other components.
The bioactive glass provided by the invention contains 18.0% -22.0% of Na 2 O according to the amount of oxide substances, and is beneficial to improving the activity of the bioactive glass by matching with other components.
The bioactive glass provided by the invention can be used for preventing decayed teeth, resisting decayed teeth, repairing corrosion, serving as a sealing agent for holes and cracks and the like, and can be used for, but not limited to, remineralizing dental structures, serving as a dentin sealing agent, remineralizing enamel, remineralizing initial decayed teeth and remineralizing decayed dentin; it may also be included in toothpastes, mouthwashes, gels, restorative materials, and the like, or used to reduce dentin sensitivity, and/or enhance tissue engagement, and the like.
The bioactive glass provided by the invention can be incorporated into toothpastes, mouthwashes, dentifrices, chewing gums, gels, and the like for use in the oral cavity. The bioactive glass provided by the invention can be used for repairing bones or skin as a material or a preparation or a composition for repairing bones or skin.
The bioactive glass provided by the invention can be applied topically, such as by preparing it as an emulsion, lotion, ointment, powder, gel or paste for application to teeth or skin; such as toothpaste that can be prepared to include bioactive glass for application to the teeth of a patient suffering from tooth decay, periodontal disease, sensitive teeth, etc.; it can be used for treating periodontal disease, preventing and/or treating dental caries; it also can increase the deposition rate of hydroxyapatite to close the surface of dentinal tubules, and can be used for treating dental hypersensitivity.
The bioactive glass of the present invention may be formulated with other necessary adjuvants to form a composition for use in the various formulations or applications described above. The auxiliary agent may be any component other than the bioactive glass, including but not limited to a component added to prepare the composition into a form suitable for use, a component to make the composition more stable for a long period of time, and the like.
The bioactive glass of the present invention or a composition comprising the bioactive glass may also comprise one or more antimicrobial agents, one or more tartar control agents, and one or more structure-building agents.
In the composition, the bioactive glass may be present in an amount of 0.1% to 50.0% based on the total mass of the composition. In some embodiments, the bioactive glass is present in the composition in an amount of 1.0% to 20.0% based on the total mass of the composition. In some embodiments, the bioactive glass is present in the composition in an amount of 1.0% to 10.0% based on the total mass of the composition. The adjuvants may include fillers, lubricants and/or binders and the like.
In some embodiments, a composition comprising the aforementioned bioactive glass and an adjunct, further comprising an antimicrobial agent, a tartar control agent, a structure-building agent, or a combination thereof; the bioactive glass is present in an amount of 0.1% to 50.0% based on the total mass of the composition; the composition is in the form of emulsion, lotion, ointment, powder, gel or paste.
The bioactive glass of the present invention or a composition comprising the bioactive glass of the present invention can be used in a method for preventing or treating dental hypersensitivity, a method for partially or totally occluding dentinal tubules, a method for preventing incipient caries, a method for preventing or treating tooth decay, a method for remineralizing incipient caries, a method for remineralizing enamel, a method for occluding cracks in a tooth structure, a method for occluding gaps in a tooth structure, a method for lining a tooth structure, a method for covering dental pulp, or/and a method for treating a tooth structure after periodontal surgery. In some embodiments, the bioactive glass of the present invention or a composition comprising the bioactive glass of the present invention may be used in a method for preventing or treating dental hypersensitivity, a method for partially or fully occluding dentinal tubules, a method for incipient caries remineralization, a method for occluding a crack in a tooth structure, or a method for occluding a point crack in a tooth structure. In some embodiments, the bioactive glass of the present invention or a composition comprising the bioactive glass of the present invention can be used in a method of partially or fully occluding dentinal tubules, in a method of occluding a fissure of a dental structure, or in a method of occluding a point gap of a dental structure.
The bioactive glass of the present invention or a composition comprising the bioactive glass of the present invention may be used in fields including, but not limited to, dental restoration, bone restoration, skin restoration, and/or as a pharmaceutical carrier.
A method for preventing or treating tooth decay comprising contacting a tooth structure with an effective amount of bioactive glass. A method for preventing incipient caries comprising contacting a dental structure with an effective amount of bioactive glass. A method of treating dental hypersensitivity comprising contacting one or more sensitive teeth with an effective amount of said bioactive glass. A method of partially or fully occluding a dentin tubule comprising contacting the tubule with an effective amount of a bioactive glass. A method of remineralizing enamel comprising contacting a tooth structure with an effective amount of bioactive glass. A method of incipient caries remineralization comprising contacting a tooth structure with an effective amount of bioactive glass. A method of sealing a fissure in a dental structure comprising contacting the dental structure with an effective amount of bioactive glass. A method of closing a dental structure spot gap comprising contacting a dental structure with an effective amount of bioactive glass. A method of lining a dental structure comprising contacting the dental structure with an effective amount of bioactive glass. A method of covering dental pulp comprising contacting a dental structure with an effective amount of bioactive glass. A method of treating a periodontal postoperative dental structure comprising contacting the dental structure with an effective amount of bioactive glass. A method of repairing bone or skin comprising contacting the bone or skin to be repaired with an effective amount of bioactive glass.
The bioactive glass provided by the invention can be mineralized more quickly, and can better prevent, relieve and/or radically cure symptoms such as tooth allergy, decayed tooth and the like when being applied to teeth. The bioactive glass has the advantages of enhanced bioactivity, rapid deposition rate of hydroxyapatite, rapid wound healing rate, mineralization rate higher than 45S5, rapid formation of hydroxyapatite, and rapid occlusion of dentinal tubules, and alleviation/radical treatment of dental hypersensitivity symptoms.
Remineralization refers to any formation of hydroxyapatite.
The term "dental structure" refers to all parts of a tooth including, but not limited to, enamel, dentin, medulla, root structure, cementum, root, crown, all dental artifacts, and the like.
For the purposes of the present invention, the tissue may be bone tissue, cartilage, soft tissue including connective tissue, and dental tissue including calcified dental tissue such as enamel and dentin.
The bioactive glass of the invention can be prepared according to the following method, which comprises the following steps:
1) Weighing the raw materials of all the components according to the formula proportion, uniformly mixing, and filling into a crucible;
2) Placing the crucible in an electric furnace, setting the temperature rising speed of the electric furnace to be between 400 and 450 ℃ within 0.5 to 1.5 hours, then to be between 900 and 950 ℃ within 0.5 to 1.5 hours, then to be between 1300 and 1400 ℃ within 1.5 to 2.5 hours, and finally preserving the heat for 1 to 4 hours at 1300 to 1400 ℃ to melt and clarify the glass liquid to obtain molten glass liquid;
3) Quenching the molten glass liquid with water to obtain bioactive glass; optionally include
4) And (3) drying the obtained bioactive glass in a drying oven at 100-120 ℃ for 4-8 hours, ball milling for 2-8 hours (absolute ethyl alcohol is used as a medium, the rotating speed is 150-500 r/min), sieving with a 400-600 target standard sieve, and drying at 100-120 ℃ for 2-6 hours to obtain the bioactive glass.
In some embodiments, the bioactive glass of the present invention can be prepared according to a method comprising the steps of:
1) Weighing the raw materials of the components according to the formula proportion, uniformly mixing in a mortar, and loading into a corundum crucible;
2) Placing the crucible in a high-temperature electric furnace at room temperature, setting the heating speed of the electric furnace to be 1h to be heated to 400-450 ℃, setting the heating speed of the electric furnace to be 1h to be heated to 900-950 ℃, and slowly heating the crucible to 1300-1400 ℃ for 2h to fully decompose and melt the component raw materials, and finally preserving the heat for 2h at 1300-1400 ℃ to melt and clarify the glass liquid to obtain molten glass liquid;
3) Directly water-quenching the molten glass liquid to obtain bioactive glass; optionally include
4) And (3) drying the obtained bioactive glass particles in a baking oven at 110 ℃ for 6 hours, ball milling by using a planetary ball mill (the medium is absolute ethyl alcohol, the rotating speed is 300 r/min), sieving by using a 500-mesh standard sieve, and drying at 110 ℃ for 4 hours to obtain the bioactive glass.
The method for preparing the bioactive glass is easy to control and implement and can obtain the product meeting the requirements.
Drawings
FIG. 1 shows XRD (X-ray powder diffraction) patterns of bioactive glass powder samples after 24 hours of culture in simulated body fluid, wherein characteristic peak intensities are from high to low, and are respectively a detection pattern of example 2, a detection pattern of example 3 and a standard pattern of hydroxyapatite of comparative example 1.
FIG. 2 is a sample surface SEM (scanning electron microscope) photograph of human tooth samples cultured for 3d, 7d and 14d in simulated body fluid after simulated tooth brushing of a 1% strength solution of the bioactive glass purified water of example 2.
FIG. 3 is a SEM photograph of the sample surface of human tooth samples cultured for 3d, 7d and 14d in simulated body fluids after simulated tooth brushing with a 1% strength solution of the bioactive glass purified water of example 3.
FIG. 4 is a SEM photograph of the sample surface of a human tooth sample cultured for 3d, 7d and 14d in a simulated body fluid after simulated tooth brushing of a 1% strength solution of the bioactive glass purified water of comparative example 1.
Fig. 5 is a SEM image of the sample surface of human tooth samples incubated 3d, 7d and 14d in simulated body fluid.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are shown in the tables. The embodiments described below by referring to the tables are exemplary and intended to illustrate the present invention and should not be construed as limiting the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. All patents and publications referred to herein are incorporated by reference in their entirety. The terms "comprising" or "including" are used in an open-ended fashion, i.e., including the teachings described herein, but not excluding additional aspects. In the present invention, all numbers disclosed herein are approximate, whether or not the word "about" or "about" is used. The numerical value of each number may vary by + -10% or less or by a reasonable amount as recognized by one of ordinary skill in the art, such as a 1%, 2%, 3%, 4% or 5% difference.
The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
All temperatures are given in degrees celsius in the examples described below, unless otherwise indicated. The reagents used are all commercially available or can be prepared by the methods described herein.
The following abbreviations are used throughout the present invention: wt.% means mass percent; DEG C, SEM, scanning electron microscope, XRD, X-ray powder diffraction, μm, micrometer, ml, milliliter, r/min, revolutions per minute;
referring to time, d represents day, h represents hour, min represents minute, and s represents second.
In the present invention, room temperature refers to the ambient temperature, which may be from 0℃to 45 ℃. In some embodiments, the room temperature is from 10 ℃ to 30 ℃. In some embodiments, the room temperature is 20 ℃ to 35 ℃. In some embodiments, the room temperature is 20 ℃ to 30 ℃.
In the following examples, pure water used therein was boiled.
Example 1: testing of crystallization amount:
Weighing 0.2g of active glass powder, adding into 100ml of Simulated Body Fluid (SBF), placing in a constant temperature shaking table at 37 ℃, starting a reciprocating mode, rotating at 120r/min, taking out after 24 hours, filtering, cleaning, drying, mixing uniformly, and testing the percentage content of crystals by XRD.
The simulated body fluid composition is as follows:
Preparing simulated body fluid: prepared with reference to the ISO/TR 10271 standard, pH was adjusted to 7.0 with NaOH (sodium hydroxide) aqueous solution; wherein the pure water is boiled and sterilized, all vessels are sterilized at 121 ℃ and the prepared simulated body fluid is stored in a sealed manner for 1 week.
The inventor finds from experiments that: the crystallization level can reflect the speed of the used glass for generating the hydroxyapatite under the same condition to a certain extent, the crystallization level is high, the biological activity of the glass is high, but XRD (X-ray diffraction) calculation crystallization level is not the only index of the reaction activity because XRD can only semi-quantitatively calculate the crystallization level of the glass, and the biological activity of the glass needs to be compared with the test result of SEM (X-ray diffraction). In order to preliminarily screen glass components with better biological activity, the inventor changes the components and/or the content of the components by researching on the basic formula 45S5, then detects the crystallization amount of the obtained glass, and preliminarily judges the important components and the content range thereof by the component change and the crystallization amount change, wherein the components are calculated according to the mass (wt%) of oxide.
Table 1: group A bioglass component and amount of hydroxyapatite produced
Table 2: group B bioglass component and amount of hydroxyapatite produced
Table 3: group C bioglass component and amount of hydroxyapatite produced
Table 4: d group bioglass component and amount of hydroxyapatite produced
As can be seen from the crystallization amounts shown in tables 1to 4, the introduction of different amounts of Li 2 O and/or CaF 2 into the base glass 45S5, respectively, has found that the crystallization amount after hydration can be increased within a certain range, but the crystallization amount is decreased again after a certain range. From tables 1to 4, it was found that when the bioactive glass had a CaF 2 of 5.55 to 7.66% and a Li 2 O of 0.84 to 1.25% and a mass ratio of Li 2 O to CaF 2 of 0.11 to 0.16, the crystallization amount was high, and the bioactive glass was more advantageous in improving the activity.
Example 2
According to the amount of the compound, the raw materials 28.4％SiO2,7.6％P2O5,26.2％Na2CO3,27.6％CaCO3,5.6％CaF2,1.5％Li2CO3,2.1％MgO,1.0％BaCO3 of chemical purity are added into a mortar, mixed uniformly and filled into a corundum crucible. Placing the corundum crucible in a high-temperature electric furnace at room temperature, setting the heating speed of the electric furnace to be 1h to 400 ℃, setting the heating speed to be 1h to 900 ℃, and then slowly heating to 1350 ℃ for 2h to fully decompose and melt each batch, and finally preserving the heat for 2h at 1350 ℃ to fully melt and clarify the molten glass; and (3) directly water-quenching the molten glass liquid to obtain granular bioactive glass particles. And (3) drying the obtained bioactive glass particles in a baking oven at 110 ℃ for 6 hours, ball-milling for 4 hours by using a planetary ball mill (the medium is absolute ethyl alcohol, the rotating speed is 300 r/min), and then sieving by using a 500-target standard sieve, and drying for 4 hours at 110 ℃ to obtain the bioactive glass particles with a certain particle size.
Example 3
According to the amount of the compound, the raw materials 29.1％SiO2,8.0％P2O5,27.5％Na2CO3,28.9％CaCO3,2.5％CaF2,1.6％Li2CO3,1.3％MgO,0.5％BaCO3 of chemical purity are added into a mortar, mixed uniformly and filled into a corundum crucible. Placing the corundum crucible in a high-temperature electric furnace at room temperature, setting the heating speed of the electric furnace to be 1h to 400 ℃, setting the heating speed to be 1h to 900 ℃, and then slowly heating to 1350 ℃ for 2h to fully decompose and melt each batch, and finally preserving the heat for 2h at 1350 ℃ to fully melt and clarify the molten glass; and (3) directly water-quenching the molten glass liquid to obtain granular bioactive glass particles. And (3) drying the obtained bioactive glass particles in a baking oven at 110 ℃ for 6 hours, ball-milling for 4 hours by using a ball mill (the medium is absolute ethyl alcohol, the rotating speed is 300 r/min), sieving by using a 500-mesh standard sieve, and drying at 110 ℃ for 4 hours to obtain the bioactive glass particles with certain particle size.
Comparative example 1 (i.e., 45S5 formulation):
According to the mass of the compound, adding 33.01% of SiO 2,4.44％P2O5,30.48％Na2CO3,32.07％CaCO3 which is a chemically pure raw material into a mortar, uniformly mixing, and loading into a corundum crucible. Placing the corundum crucible in a high-temperature electric furnace at room temperature, setting the heating speed of the electric furnace to be 1h to 400 ℃, setting the heating speed to be 1h to 900 ℃, and then slowly heating to 1350 ℃ for 2h to fully decompose and melt each batch, and finally preserving the heat for 2h at 1350 ℃ to fully melt and clarify the molten glass; and (3) directly water-quenching the molten glass liquid to obtain granular bioactive glass particles. And (3) drying the obtained bioactive glass particles in a baking oven at 110 ℃ for 6 hours, ball-milling for 4 hours by using a ball mill (the medium is absolute ethyl alcohol, the rotating speed is 300 r/min), sieving by using a 500-target standard sieve, and drying for 4 hours to obtain the bioactive glass particles with a certain particle size.
Example 4: activity test
1. XRD testing
Ball milling, sieving and drying the obtained bioactive glass particles, and respectively measuring samples with 500 meshes by using a Markov 2000 laser particle sizer to ensure that the particle sizes are in the same range, wherein the particle size distribution of each sample is shown in Table 5; then weighing the same amount of 0.2g, placing in 100ml of SBF (simulated body fluid), and culturing for 24 hours at 37 ℃ in a constant-temperature oscillating water bath; the sample was then transferred to filter paper and filtered, the sample left on the filter paper was repeatedly rinsed with absolute ethanol, after the filtration was completed, the sample was placed in an oven at 110 ℃, dried for 4 hours and then placed in a dryer for cooling. The cooled sample is peeled off from the filter paper, ground in an agate mortar for 5min, fully and uniformly mixed, and then the sample is characterized by XRD to determine whether the generated product is hydroxyapatite and the peak intensity of the characteristic peak.
Table 5: particle size distribution of each sample
| Sample of | D10(μm) | D50(μm) | D90(μm) |
| Example 2 | 3.452 | 7.137 | 14.419 |
| Example 3 | 2.987 | 6.662 | 14.870 |
| Comparative example 1 | 2.942 | 6.539 | 13.957 |
The XRD detection results are shown in figure 1. The spectra showed that the substances produced in example 2, example 3 and comparative example 1 were all hydroxyapatite crystal phases. And under the same conditions, the crystallization amount of the hydroxyapatite contained in the example 2 and the example 3 is obviously higher than 45S5 of the comparative example 1.
2. SEM test
The isolated human teeth are transversely cut into sheet-shaped samples with the thickness of 2.5mm, the cut samples of each tooth are separately placed, the difference between different teeth is avoided, the teeth are ground and polished by a precise grinding and polishing machine, and firstly, 6% citric acid aqueous solution (mass concentration) is used for corroding, so that dentin tubules are exposed, and the human teeth samples are obtained.
The human tooth samples were simulated to brush teeth with 1% (mass concentration) water (pure water) solutions of the bioactive glasses of examples and comparative examples, respectively, each side was brushed for 30 seconds, and after brushing teeth, placed in a beaker to be rinsed 3 times with pure water, and then soaked with 100ml of SBF (simulated body fluid); repeating the above steps 1 time every day for 12 hours, and changing the simulated body fluid at the same time every day (e.g. 8:00 a.m. and 20:00 a.m. each 1 time each, 8:00 a.m. the simulated body fluid is changed); samples were taken at the same time after 3 days, 7 days, and 14 days (e.g., 8:00 a.m. after 3 days, 8:00 a.m. after 7 days, 8:00 a.m. after 14 days), sonicated with absolute ethanol for 15min and dried in the shade for SEM testing.
SEM test results are shown in fig. 2-5. As is clear from the SEM image, in experimental example 2, the dentin pinholes were observed to have a tendency to be formed around hydroxyapatite at 3d and a large part of the dentin pinholes were closed at 7d under the same culture conditions, and the sample of example 3 was slightly slower in the restoration of dentin pinholes than the sample of example 2, but more dentin pinholes were also closed at 7 d. Whereas in comparative example 1, a part of dentin pinholes was closed at 14 d.
The bioactive glass of comparative example 1, example 2 and example 3 showed a larger amount of devitrification than that of comparative example 1, i.e., more hydroxyapatite crystals were produced in example 2 and example 3 under the same conditions as measured by XRD. Under the same conditions, the bioactive glasses of example 2 and example 3 were tested by SEM to close more dentinal tubules at 14d, i.e., repair dentinal tubules faster, than the bioactive glass of comparative example 1. By combining XRD and SEM test results of comparative example 1, example 2 and example 3, under the same conditions, the produced hydroxyapatite crystals are more, and the closed dentin tubules are more, namely the activity of the bioactive glass of example 2 and example 3 is obviously better than that of comparative example 1, so that the dental hypersensitivity symptoms can be quickly relieved and radically cured, and the effect is durable.
While the methods of this invention have been described in terms of preferred embodiments, it will be apparent to those of skill in the art that variations and combinations of the methods and applications described herein can be made and applied within the spirit and scope of the invention. Those skilled in the art can, with the benefit of this disclosure, suitably modify the process parameters to achieve this. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and are deemed to be included within the present invention.
Claims (10)
1. A bioactive glass comprising the following components in terms of oxide mass:
Wherein the mass ratio of Li 2 O to CaF 2 is 0.11-0.16.
2. A bioactive glass comprises ：SiO237.4％、P2O59.95％、Na2O 20.36％、CaO 20.36％、CaF2 7.37％、Li2O 0.81％、MgO 2.72％ and BaO 1.03% by weight of oxide; or SiO237.24％、P2O59.92％、Na2O 20.29％、CaO20.29％、CaF2 7.35％、Li2O 1.21％、MgO 1.63％ and BaO 2.06%; or SiO237.43％、P2O510.02％、Na2O 20.19％、CaO 20.38％、CaF27.38％、Li2O 0.80％、MgO 2.77％ and BaO 1.02%.
3. Use of the bioactive glass of claim 1 or 2 in the preparation of a toothpaste, mouthwash, dentifrice, chewing gum, gel, or pharmaceutical carrier.
4. Use of a bioactive glass as claimed in claim 1 or 2 in the preparation of a composition for use in a method of preventing or treating dental hypersensitivity, for partially or totally occluding dentinal tubules, for use in a method of preventing incipient caries, for use in a method of preventing or treating caries, for use in a method of incipient caries remineralization, for use in remineralizing enamel, for use in a method of occluding a crack in a tooth structure, for use in a method of occluding a point gap in a tooth structure, for use in a method of lining a tooth structure, for use in a method of covering dental pulp, or/and for use in a method of treating a tooth structure after periodontal surgery, or for use in skeletal repair.
5. A composition comprising the bioactive glass of claim 1 or 2 and an adjunct, wherein the composition is used in a method for preventing or treating dental hypersensitivity, a method for partially or totally occluding dentinal tubules, a method for preventing incipient caries, a method for preventing or treating caries, a method for incipient caries remineralization, a method for remineralizing enamel, a method for occluding a crack in a tooth structure, a method for occluding a point gap in a tooth structure, a method for lining a tooth structure, a method for covering dental pulp, or/and a method for treating a tooth structure after periodontal surgery.
6. The composition of claim 5 which is an emulsion, lotion, ointment, powder, gel or paste.
7. The composition of claim 5, wherein the bioactive glass is present in an amount of 0.1% to 50.0% based on the total mass of the composition.
8. The composition of claim 5, further comprising an antibacterial agent, a tartar control agent, a structure-building agent, or a combination thereof.
9. A method of making the bioactive glass of claim 1 or 2, comprising the steps of:
1) Weighing the raw materials of all the components according to the formula proportion, uniformly mixing, and filling into a crucible;
2) Placing the crucible in an electric furnace, setting the temperature rising speed of the electric furnace to be between 400 and 450 ℃ within 0.5 to 1.5 hours, then setting the temperature rising speed to be between 900 and 950 ℃ within 0.5 to 1.5 hours, then heating to be between 1300 and 1400 ℃ within 1.5 to 2.5 hours, and finally preserving the heat for 1 to 4 hours at the temperature of between 1300 and 1400 ℃ to melt and clarify the glass liquid to obtain molten glass liquid;
3) And (5) water quenching the molten glass liquid to obtain the bioactive glass.
10. The method of claim 9, further comprising:
4) Drying the obtained bioactive glass particles in an oven at 100-120 ℃ for 4-8 hours, and then ball milling for 2-8 hours by using a planetary ball mill, wherein the medium is absolute ethyl alcohol, and the rotating speed is 150-500 r/min; sieving with 400-600 target standard sieve, and baking at 100-120 deg.c for 2-6 hr to obtain bioactive glass.
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