CN111110576B - 一种牙釉质再生组合物的制备方法 - Google Patents
一种牙釉质再生组合物的制备方法 Download PDFInfo
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- CN111110576B CN111110576B CN202010089792.XA CN202010089792A CN111110576B CN 111110576 B CN111110576 B CN 111110576B CN 202010089792 A CN202010089792 A CN 202010089792A CN 111110576 B CN111110576 B CN 111110576B
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- Prior art keywords
- oil
- water
- calcium
- phosphate
- mixture
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- 210000003298 dental enamel Anatomy 0.000 title claims abstract description 58
- 239000000203 mixture Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 230000008929 regeneration Effects 0.000 title claims abstract description 9
- 238000011069 regeneration method Methods 0.000 title claims abstract description 9
- 239000007764 o/w emulsion Substances 0.000 claims abstract description 54
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 48
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 46
- 159000000007 calcium salts Chemical class 0.000 claims abstract description 42
- 239000007787 solid Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002324 mouth wash Substances 0.000 claims abstract description 35
- 229940051866 mouthwash Drugs 0.000 claims abstract description 35
- 229940034610 toothpaste Drugs 0.000 claims abstract description 35
- 239000000606 toothpaste Substances 0.000 claims abstract description 35
- 239000010452 phosphate Substances 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 31
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 26
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims abstract description 18
- 230000008439 repair process Effects 0.000 claims abstract description 17
- 239000003921 oil Substances 0.000 claims description 43
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 42
- 235000019198 oils Nutrition 0.000 claims description 42
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 40
- 238000002156 mixing Methods 0.000 claims description 37
- 239000012071 phase Substances 0.000 claims description 28
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- 239000007762 w/o emulsion Substances 0.000 claims description 23
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 22
- 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 claims description 22
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 21
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims description 21
- -1 phosphate radical Chemical class 0.000 claims description 20
- 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 claims description 18
- 241000196324 Embryophyta Species 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 15
- 239000001506 calcium phosphate Substances 0.000 claims description 13
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 13
- 235000011010 calcium phosphates Nutrition 0.000 claims description 13
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 13
- 239000000377 silicon dioxide Substances 0.000 claims description 13
- 239000008346 aqueous phase Substances 0.000 claims description 12
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- 239000011787 zinc oxide Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000004408 titanium dioxide Substances 0.000 claims description 11
- 229910021536 Zeolite Inorganic materials 0.000 claims description 10
- 229960000892 attapulgite Drugs 0.000 claims description 10
- 239000000378 calcium silicate Substances 0.000 claims description 10
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 10
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 10
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 10
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims description 10
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 10
- 229910001701 hydrotalcite Inorganic materials 0.000 claims description 10
- 229960001545 hydrotalcite Drugs 0.000 claims description 10
- 239000000944 linseed oil Substances 0.000 claims description 10
- 235000021388 linseed oil Nutrition 0.000 claims description 10
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 10
- 239000001095 magnesium carbonate Substances 0.000 claims description 10
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 10
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 10
- 239000000347 magnesium hydroxide Substances 0.000 claims description 10
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 10
- 239000010445 mica Substances 0.000 claims description 10
- 229940043356 mica Drugs 0.000 claims description 10
- 229910052618 mica group Inorganic materials 0.000 claims description 10
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 10
- 229910052625 palygorskite Inorganic materials 0.000 claims description 10
- 239000004094 surface-active agent Substances 0.000 claims description 10
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 10
- 239000010457 zeolite Substances 0.000 claims description 10
- 235000019484 Rapeseed oil Nutrition 0.000 claims description 9
- 239000000839 emulsion Substances 0.000 claims description 9
- 239000004006 olive oil Substances 0.000 claims description 9
- 235000008390 olive oil Nutrition 0.000 claims description 9
- 235000012239 silicon dioxide Nutrition 0.000 claims description 9
- 235000019483 Peanut oil Nutrition 0.000 claims description 8
- 239000005313 bioactive glass Substances 0.000 claims description 8
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002105 nanoparticle Substances 0.000 claims description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 8
- 239000000312 peanut oil Substances 0.000 claims description 8
- 239000003549 soybean oil Substances 0.000 claims description 8
- 235000012424 soybean oil Nutrition 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 claims description 7
- 229910000020 calcium bicarbonate Inorganic materials 0.000 claims description 7
- 239000004227 calcium gluconate Substances 0.000 claims description 7
- 229960004494 calcium gluconate Drugs 0.000 claims description 7
- 235000013927 calcium gluconate Nutrition 0.000 claims description 7
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 claims description 7
- 239000003240 coconut oil Substances 0.000 claims description 7
- 235000019864 coconut oil Nutrition 0.000 claims description 7
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 7
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 7
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 7
- 239000004925 Acrylic resin Substances 0.000 claims description 6
- 239000004254 Ammonium phosphate Substances 0.000 claims description 6
- 235000019482 Palm oil Nutrition 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 6
- 235000019498 Walnut oil Nutrition 0.000 claims description 6
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 6
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 6
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 6
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 6
- 239000000920 calcium hydroxide Substances 0.000 claims description 6
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 6
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 claims description 6
- 239000001527 calcium lactate Substances 0.000 claims description 6
- 229960002401 calcium lactate Drugs 0.000 claims description 6
- 235000011086 calcium lactate Nutrition 0.000 claims description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000292 calcium oxide Substances 0.000 claims description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 6
- 239000010495 camellia oil Substances 0.000 claims description 6
- 239000001913 cellulose Substances 0.000 claims description 6
- 229920002678 cellulose Polymers 0.000 claims description 6
- 235000005687 corn oil Nutrition 0.000 claims description 6
- 239000002285 corn oil Substances 0.000 claims description 6
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 6
- 229910000396 dipotassium phosphate Inorganic materials 0.000 claims description 6
- 235000019797 dipotassium phosphate Nutrition 0.000 claims description 6
- 125000000524 functional group Chemical group 0.000 claims description 6
- 239000008169 grapeseed oil Substances 0.000 claims description 6
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 6
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 6
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 6
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 6
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 6
- 239000002540 palm oil Substances 0.000 claims description 6
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 6
- 229920000573 polyethylene Polymers 0.000 claims description 6
- 239000008159 sesame oil Substances 0.000 claims description 6
- 235000011803 sesame oil Nutrition 0.000 claims description 6
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 6
- 239000001488 sodium phosphate Substances 0.000 claims description 6
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 6
- 235000011008 sodium phosphates Nutrition 0.000 claims description 6
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 6
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 6
- 239000008170 walnut oil Substances 0.000 claims description 6
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- 239000004793 Polystyrene Substances 0.000 claims description 5
- 241000270295 Serpentes Species 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 229920002223 polystyrene Polymers 0.000 claims description 5
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 5
- 235000011009 potassium phosphates Nutrition 0.000 claims description 5
- 229920002545 silicone oil Polymers 0.000 claims description 5
- 241001465754 Metazoa Species 0.000 claims description 4
- 235000006484 Paeonia officinalis Nutrition 0.000 claims description 4
- 244000170916 Paeonia officinalis Species 0.000 claims description 4
- 229960003237 betaine Drugs 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 4
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- 150000001875 compounds Chemical class 0.000 claims description 4
- 239000007822 coupling agent Substances 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 4
- 235000010755 mineral Nutrition 0.000 claims description 4
- 239000011707 mineral Substances 0.000 claims description 4
- 239000002736 nonionic surfactant Substances 0.000 claims description 4
- 239000012188 paraffin wax Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 239000003760 tallow Substances 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 230000000474 nursing effect Effects 0.000 claims description 3
- 239000001293 FEMA 3089 Substances 0.000 claims description 2
- 235000015278 beef Nutrition 0.000 claims description 2
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- 235000021323 fish oil Nutrition 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 6
- 239000006185 dispersion Substances 0.000 claims 4
- 239000011159 matrix material Substances 0.000 claims 3
- 229920001503 Glucan Polymers 0.000 claims 1
- 229930182470 glycoside Natural products 0.000 claims 1
- 150000002338 glycosides Chemical class 0.000 claims 1
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- 239000005909 Kieselgur Substances 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 5
- JXRVKYBCWUJJBP-UHFFFAOYSA-L calcium;hydrogen sulfate Chemical compound [Ca+2].OS([O-])(=O)=O.OS([O-])(=O)=O JXRVKYBCWUJJBP-UHFFFAOYSA-L 0.000 description 5
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- 210000003296 saliva Anatomy 0.000 description 4
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 4
- 239000003765 sweetening agent Substances 0.000 description 4
- 239000002562 thickening agent Substances 0.000 description 4
- 241000779819 Syncarpia glomulifera Species 0.000 description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-M dihydrogenphosphate Chemical compound OP(O)([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-M 0.000 description 3
- 239000001739 pinus spp. Substances 0.000 description 3
- 229940036248 turpentine Drugs 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 2
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
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- 241000857235 Dieteria Species 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
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- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 1
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- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 1
- SNRUBQQJIBEYMU-NJFSPNSNSA-N dodecane Chemical group CCCCCCCCCCC[14CH3] SNRUBQQJIBEYMU-NJFSPNSNSA-N 0.000 description 1
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical group CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
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- 229920000592 inorganic polymer Polymers 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
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- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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Abstract
一种牙釉质再生组合物的制备方法，本发明通过将可溶性钙盐和可溶性磷酸盐分别作为固体粒子稳定的水包油包水乳液的内水相进行包裹，加入牙膏、牙釉质修复凝胶或者漱口水中。这样制得的牙膏、牙釉质修复凝胶或者漱口水中的可溶性钙盐和可溶性磷酸盐能够同时长时间稳定存在。当使用本发明的牙膏、牙釉质修复凝胶或者漱口水时，固体粒子稳定的水包油包水乳液在摩擦、挤压等作用下破裂，释放出内水相中包裹的可溶性钙盐和可溶性磷酸盐，使口腔液体中含有较高浓度的钙离子和磷酸根离子，能够提高牙釉质再矿化的速率。
Description
技术领域
本发明属于日化以及口腔硬组织医疗、护理、清洁领域，具体涉及医疗及口腔清洁护理的牙釉质再生组合物及其制备方法。
背景技术
牙釉质是人体最坚硬的组织。成熟的牙釉质按重量计包含大约96％的羟基磷灰石、3％的水以及1％的蛋白质和脂类。作为牙齿的最外层，牙釉质承受着咬合、磨擦、磨损以及来自饮食和细菌产生的酸蚀等各种物理和化学侵蚀。一般而言，羟基磷灰石在pH＜5.5时溶解导致牙釉质的脱矿问题。
唾液中含有一定浓度的钙离子和磷酸根离子，能够在一定程度上缓冲唾液pH值的变化，从而抑制羟基磷灰石的溶解。在pH＞5.5和钙离子、磷离子浓度较高时，唾液中有磷酸钙生成，使脱矿牙齿得以再矿化。通常情况下，唾液中所含钙离子和磷酸根离子的浓度较低，难以形成足够量的羟基磷灰石来修复脱矿的牙釉质。
牙膏、牙釉质修复凝胶或者漱口水中添加钙盐和磷酸盐，可以提高使用时口腔中的钙离子浓度和磷酸根离子浓度，有利于牙齿再矿化过程。然而，当给牙膏、牙釉质修复凝胶或者漱口水中直接添加溶解度较小的钙盐和磷酸盐时，所能够提供的钙离子浓度和磷酸根离子浓度较低。如果给牙膏、牙釉质修复凝胶或者漱口水中添加溶解度较大的钙盐和磷酸盐时，由于磷酸钙、磷酸氢钙和羟基磷灰石等的溶度积较小，牙膏中的钙离子和磷酸根离子迅速反应形成沉淀，使得牙膏、牙釉质修复凝胶或者漱口水所含游离钙离子和磷酸根离子浓度依然较低。因此，直接给牙膏、牙釉质修复凝胶或者漱口水中添加钙盐和磷酸盐，能够提供的游离钙离子和磷酸根离子浓度较低，在有限的使用时间和使用频率时在牙釉质上再矿化的速率有限。
发明内容
本发明的目的在于提供一种能够使口腔液体中含有较高浓度的钙离子和磷酸根离子，能够提高牙釉质再矿化速率的牙釉质再生组合物的制备方法。
为达到上述目的，本发明采用的技术方案是：
1)制备固体粒子稳定的含有可溶性钙盐的水包油包水乳液：
将用于制备固体稳定乳液的有机、无机微纳米粒子或其混合物的固体粒子按0.1～25：100的质量比加入到用于口腔治疗的水剂、凝胶剂、制备牙膏、漱口水或者牙釉质修复凝胶用的所有植物来源、动物来源、矿物来源的天然油脂中、或者以石油化工产品及天然提取原料加工的合成油脂中加热至30℃～80℃搅拌均匀形成油相；
将能够溶解于水、醇类物质并能够产生游离态钙离子的物质加入水中，制成钙离子浓度为0.1％～60％的水溶液，将水溶液和油相按0.5：9.5～1.5：0.5的体积比混合后置于高速分散机上加热至30℃～80°以10转/分至24000转/分搅拌0.5分钟～120分钟得到油包水乳液；
将用于制备固体稳定乳液的有机、无机微纳米粒子或其混合物的固体粒子按0.1～25：100的质量比加入加入水中，得到水相溶液，将油包水乳液与水相溶液按0.5：9.5至1.5：0.5的体积比混合后置于高速分散机上加热至30℃～80°以10转/分至24000转/分搅拌0.5分钟～120分钟得到含有可溶性钙盐的水包油包水乳液；
2)制备固体粒子稳定的含有可溶性磷酸盐的水包油包水乳液：
将用于制备固体稳定乳液的有机、无机微纳米粒子或其混合物的固体粒子按0.1～25：100的质量比加入到用于口腔治疗或者制备牙膏、漱口水或者牙釉质修复凝胶用的所有植物来源、动物来源或者矿物来源的天然油脂，或者以石油化工产品及天然提取原料加工的合成油脂中加热至30℃～80℃搅拌均匀形成油相；
将能够提供游离态磷酸根、磷酸氢根或磷酸二氢根离子的化合物加入水中，制成磷酸根、磷酸氢根或磷酸二氢根离子浓度不0.1％～60％的水溶液，将水溶液和油相按0.5：9.5～1.5：0.5的体积比混合后置于高速分散机上加热至30℃～80°以10转/分至24000转/分搅拌0.5分钟～120分钟得到油包水乳液；
将用于制备固体稳定乳液的有机、无机微纳米粒子或其混合物的固体粒子按0.1～25：100的质量比加入水中，得到水相溶液，将油包水乳液与水相溶液按0.5：9.5至1.5：0.5的体积比混合后置于高速分散机上加热至30℃～80°以10转/分至24000转/分搅拌0.5分钟～120分钟得到含有可溶性磷酸盐的水包油包水乳液；
3)同时含有可溶性钙盐和可溶性磷酸盐的漱口水、牙膏或牙釉质修复凝胶制备方法如下：
3-1)同时含有可溶性钙盐和可溶性磷酸盐的漱口水制备方法如下：
将加热至30℃～80℃的含有可溶性钙盐的水包油包水乳液、含有可溶性磷酸盐的水包油包水乳液和漱口水基质、牙膏基质或牙釉质修复凝胶基质混合，以10转/分至24000转/分搅拌0.5分钟～120分钟得到同时含有可溶性钙盐和可溶性磷酸盐的漱口水、牙膏或牙釉质修复凝胶，其中含有可溶性钙盐的水包油包水乳液所含的钙离子的物质的量与含有可溶性磷酸盐的水包油包水乳液所含磷酸根离子的物质的量的比为5：3，含有可溶性钙盐的水包油包水乳液和含有可溶性磷酸盐的水包油包水乳液与漱口水基质、牙膏基质或牙釉质修复凝胶基质的质量比为1：19至19：1。
所述步骤1、2)的固体粒子为二氧化硅、三氧化二铝、生物活性玻璃、碳酸钙、硅酸钙、磷酸钙、羟基磷灰石、氧化锌、二氧化钛、碳酸镁、氢氧化镁、硅藻土、蒙脱土、水滑石、云母、凹凸棒、沸石、聚乙烯、聚苯乙烯、聚丙烯酸类树脂、天然植物粉末及其表面改性的天然植物粉末、纤维素及其官能团两亲化衍生物中的一种或者至少两种的混合粒子；
固体粒子是经过用硅烷偶联剂、钛酸酯偶联剂、表面活性剂进行改性的二氧化硅、三氧化二铝、生物活性玻璃、碳酸钙、硅酸钙、磷酸钙、羟基磷灰石、氧化锌、二氧化钛、碳酸镁、氢氧化镁、硅藻土、蒙脱土、水滑石、云母、凹凸棒和沸石中的一种或者至少两种的混合粒子；
用于改性固体粒子的表面活性剂为用于口腔清洁护理用品的所有两亲性物质及其任意比例的组合物，包括十二烷基硫酸钠、十二烷基苯磺酸钠、月桂醇硫酸钠、葡聚糖苷类非离子表面活性剂、甜菜碱中的一种或者至少两种的混合物。
所述步骤1、2)的油脂为菜籽油、花生油、火麻油、玉米油、橄榄油、山茶油、棕榈油、葵花子油、大豆油、芝麻油、亚麻籽油、葡萄籽油、核桃油、牡丹籽油、椰子油，食用石蜡、松节油、猪油、牛油、羊油、鱼类油脂、蛙油、蛇油、有机硅油、直链烷烃类、脂类、与水不互溶的醇类中的一种或者至少两种的混合油。
所述的能够产生游离态钙离子的物质为氯化钙、碳酸钙、氢氧化钙、氧化钙、磷酸钙盐类、硝酸钙、葡萄糖酸钙、碳酸氢钙、硫酸氢钙、乳酸钙中的一种或者至少两种的混合物。
所述的能够产生游离态磷酸根、磷酸氢根、磷酸二氢根离子的化合物，包括但不仅限于磷酸钾、磷酸钠、磷酸铵、磷酸一氢钾、磷酸一氢钠、磷酸一氢铵、磷酸二氢钾、磷酸二氢钠、磷酸二氢铵的一种或者其中至少两种的混合物。
与现有技术相比本发明通过将可溶性钙盐和可溶性磷酸盐分别作为固体粒子稳定的水包油包水乳液的内水相进行包裹，加入牙膏、牙釉质修复凝胶或者漱口水中。这样制得的牙膏、牙釉质修复凝胶或者漱口水中的可溶性钙盐和可溶性磷酸盐能够同时长时间稳定存在。当使用本发明的牙膏、牙釉质修复凝胶或者漱口水时，固体粒子稳定的水包油包水乳液在摩擦、挤压等作用下破裂，释放出内水相中包裹的可溶性钙盐和可溶性磷酸盐，使口腔液体中含有较高浓度的钙离子和磷酸根离子，能够提高牙釉质再矿化的速率。
具体实施方式
下面结合实施例对本发明做进一步说明。
实施例1：
1)制备固体粒子稳定的含有可溶性钙盐的水包油包水乳液：
将0.1克二氧化硅加入100克油菜籽油中，加热至30℃搅拌均匀制得油相。然后将0.5毫升0.1％的氯化钙溶液和9.5毫升含有二氧化硅的油菜籽油加热至80℃进行混合，用高速分散机以10转/分的速率搅拌120分钟，得到油包水乳液。
将1克二氧化硅加入100克水中，制得水相。将0.5毫升制得的油包水乳液和9.5毫升水相加热至30℃进行混合，用高速分散机以24000转/分的速率搅拌0.5分钟，得到含有可溶性钙盐的水包油包水乳液。
2)制备固体粒子稳定的含有可溶性磷酸盐的水包油包水乳液：
将0.1克二氧化硅加入100克油菜籽油中，加热至80℃搅拌均匀制得油相。然后将0.5毫升0.1％的磷酸钾溶液和9.5毫升含有二氧化硅的油菜籽油加热至30℃进行混合，用高速分散机以10转/分的速率搅拌120分钟，得到油包水乳液。
将0.1克二氧化硅加入100克水中，制得水相。将0.5毫升制得的油包水乳液和9.5毫升水相加热至80℃进行混合，用高速分散机以24000转/分的速率搅拌0.5分钟，得到含有可溶性磷酸盐的水包油包水乳液。
3)制备牙膏基质
用公知的方法制备含有摩擦剂、保湿剂、表面活性剂、增稠剂、甜味剂、防腐剂、活性添加物、色素的牙膏基质。
4)制备同时含有可溶性钙盐和可溶性磷酸盐的牙膏
将0.5克含有可溶性钙盐的水包油包水乳液和含有可溶性磷酸盐的水包油包水乳液和9.5克牙膏基质加热至30℃进行混合，用高速分散机以24000转/分的速率分散0.5分钟，得到牙膏成品。这里说的含有可溶性钙盐的水包油包水乳液所含钙离子的物质的量与含有可溶性磷酸盐的水包油包水乳液所含磷酸根离子物质的量之比为5：3。
牙釉质再矿化试验表明，本实施例的牙釉质再矿化速率为普通含羟基磷灰石牙膏的52倍。
实施例2
本实施例与实施例1相同，其中不同之处在于：所用固体粒子为除二氧化硅粒子以外所有可用于口腔清洁护理用品的有机、无机、天然高分子包括但不仅限于三氧化二铝、生物活性玻璃、碳酸钙、硅酸钙、磷酸钙、羟基磷灰石、氧化锌、二氧化钛、碳酸镁、氢氧化镁、硅藻土、蒙脱土、水滑石、云母、凹凸棒、沸石、聚乙烯、聚苯乙烯、聚丙烯酸类树脂、天然植物粉末及其表面改性的天然植物粉末、纤维素及其官能团两亲化衍生物中的一种，或者为二氧化硅、三氧化二铝、生物活性玻璃、碳酸钙、硅酸钙、磷酸钙、羟基磷灰石、氧化锌、二氧化钛、碳酸镁、氢氧化镁、硅藻土、蒙脱土、水滑石、云母、凹凸棒、沸石、聚乙烯、聚苯乙烯、聚丙烯酸类树脂、天然植物粉末及其表面改性的天然植物粉末、纤维素及其官能团两亲化衍生物中至少两种的混合粒子，或者为用硅烷偶联剂、钛酸酯偶联剂、表面活性剂进行改性的二氧化硅、三氧化二铝、生物活性玻璃、碳酸钙、硅酸钙、磷酸钙、羟基磷灰石、氧化锌、二氧化钛、碳酸镁、氢氧化镁、硅藻土、蒙脱土、水滑石、云母、凹凸棒和沸石中的一种及其中至少两种的混合粒子；这里说的用于改性固体粒子的表面活性剂是十二烷基硫酸钠、十二烷基苯磺酸钠、月桂醇硫酸钠、葡聚糖苷类非离子表面活性剂、甜菜碱等中的一种或者其中至少两种的混合物；所用可溶性钙盐为可直接提供或者降解提供游离钙离子的物质包括但不仅限于碳酸钙、氢氧化钙、氧化钙、磷酸钙盐类、硝酸钙、葡萄糖酸钙、碳酸氢钙、硫酸氢钙、乳酸钙中的一种，或者氯化钙、碳酸钙、氢氧化钙、氧化钙、磷酸钙盐类、硝酸钙、葡萄糖酸钙、碳酸氢钙、硫酸氢钙、乳酸钙中的至少两种的混合物；所用可溶性磷酸盐为磷酸钠、磷酸铵、磷酸一氢钾、磷酸一氢钠、磷酸一氢铵、磷酸二氢钾、磷酸二氢钠、磷酸二氢铵中的一种，或者磷酸钾、磷酸钠、磷酸铵、磷酸一氢钾、磷酸一氢钠、磷酸一氢铵、磷酸二氢钾、磷酸二氢钠、磷酸二氢铵中的至少两种的混合物；所用油类为可用于口腔护理的一切非极性物质包括但不仅限于花生油、火麻油、玉米油、橄榄油、山茶油、棕榈油、葵花子油、大豆油、芝麻油、亚麻籽油(胡麻油)、葡萄籽油、核桃油、牡丹籽油、椰子油、食用石蜡、松节油、猪油、牛油、羊油、所有鱼类油脂、蛙油、蛇油、有机硅油、直链烷烃类、脂类、与水不互溶的醇类中的一种，或者油菜籽油、花生油、火麻油、玉米油、橄榄油、山茶油、棕榈油、葵花子油、大豆油、芝麻油、亚麻籽油(胡麻油)、葡萄籽油、核桃油、牡丹籽油、椰子油、食用石蜡、松节油、猪油、牛油、羊油、所有鱼类油脂、蛙油、蛇油、有机硅油、直链烷烃类、脂类、与水不互溶的醇类中的至少两种的混合油。
牙釉质再矿化试验表明，本实施例的牙釉质再矿化速率为普通含羟基磷灰石牙膏的32-60倍。
实施例3
1)制备固体粒子稳定的含有可溶性钙盐的水包油包水乳液：
将0.5克碳酸钙加入2克葵花籽油中，加热至80℃搅拌均匀制得油相。然后将1.5毫升60％的硝酸钙溶液和1毫升含有碳酸钙的葵花籽油加热至30℃进行混合，用高速分散机以24000转/分的速率搅拌0.5分钟，得到油包水乳液。
将1克碳酸钙加入4克水中，搅拌均匀制得水相。将1.5毫升制得的油包水乳液和1毫升水相加热至80℃进行混合，用高速分散机以300转/分的速率分散120分钟，得到含有钙离子的水包油包水乳液。
2)制备固体粒子稳定的含有可溶性磷酸盐的水包油包水乳液：
将0.5克碳酸钙加入2克葵花籽油中，加热至30℃搅拌均匀制得油相。然后将1.5毫升60％的磷酸二氢钾溶液和1毫升含有碳酸钙的葵花籽油加热至80℃进行混合，用高速分散机以24000转/分的速率搅拌0.5分钟，得到油包水乳液。
将1克碳酸钙加入4克水中，搅拌均匀制得水相。将1.5毫升制得的油包水乳液和1毫升水相加热至30℃进行混合，用高速分散机以300转/分的速率搅拌120分钟，得到含有磷酸根离子的水包油包水乳液。
3)制备牙釉质修复凝胶
用公知的方法制备含有摩擦剂、保湿剂、表面活性剂、增稠剂、甜味剂、防腐剂、活性添加物、色素的牙釉质修复凝胶。
4)制备同时含有可溶性钙盐和可溶性磷酸盐的牙釉质修复凝胶
将4克含有可溶性钙盐的水包油包水乳液和含有可溶性磷酸盐的水包油包水乳液以及0.2克牙釉质修复凝胶加热至80℃进行混合，用高速分散机以300转/分的速率搅拌120分钟，得到同时含有可溶性钙盐和可溶性磷酸盐的牙釉质修复凝胶成品。这里说的含有可溶性钙盐的水包油包水乳液所含钙离子的物质的量与含有可溶性磷酸盐的水包油包水乳液所含磷酸根离子的物质的量之比为5：3。
牙釉质再矿化试验表明，本实施例的牙釉质再矿化速率为普通含羟基磷灰石牙膏的45倍。
实施例4
本实施例与实施例3相同，其中不同之处在于：所用固体粒子为除实施例3中所用粒子外所有可用于口腔护理粒子包括但不仅限于二氧化硅、三氧化二铝、生物活性玻璃、硅酸钙、磷酸钙、羟基磷灰石、氧化锌、二氧化钛、碳酸镁、氢氧化镁、硅藻土、蒙脱土、水滑石、云母、凹凸棒、沸石、聚乙烯、聚苯乙烯、聚丙烯酸类树脂、天然植物粉末及其表面改性的天然植物粉末、纤维素及其官能团两亲化衍生物中的一种及其混合粒子，或者为二氧化硅、三氧化二铝、生物活性玻璃、碳酸钙、硅酸钙、磷酸钙、羟基磷灰石、氧化锌、二氧化钛、碳酸镁、氢氧化镁、硅藻土、蒙脱土、水滑石、云母、凹凸棒、沸石、聚乙烯、聚苯乙烯、聚丙烯酸类树脂、天然植物粉末及其表面改性的天然植物粉末、纤维素及其官能团两亲化衍生物中至少两种的混合粒子，或者为用硅烷偶联剂、钛酸酯偶联剂、表面活性剂进行改性的二氧化硅、三氧化二铝、生物活性玻璃、碳酸钙、硅酸钙、磷酸钙、羟基磷灰石、氧化锌、二氧化钛、碳酸镁、氢氧化镁、硅藻土、蒙脱土、水滑石、云母、凹凸棒和沸石中的一种及其中至少两种的混合粒子；这里说的用于改性固体粒子的表面活性剂是十二烷基硫酸钠、十二烷基苯磺酸钠、月桂醇硫酸钠、葡聚糖苷类非离子表面活性剂、甜菜碱中的一种或者其中至少两种的混合物；所用可溶性钙盐为可直接提供或者降解提供游离钙离子的物质包括但不仅限于碳酸钙、氢氧化钙、氧化钙、磷酸钙盐类、葡萄糖酸钙、碳酸氢钙、硫酸氢钙、乳酸钙中的一种，或者氯化钙、碳酸钙、氢氧化钙、氧化钙、磷酸钙盐类、硝酸钙、葡萄糖酸钙、碳酸氢钙、硫酸氢钙、乳酸钙中的至少两种的混合物；所用可溶性磷酸盐为磷酸钠、磷酸铵、磷酸一氢钾、磷酸一氢钠、磷酸一氢铵、磷酸二氢钠、磷酸二氢铵中的一种，或者磷酸钾、磷酸钠、磷酸铵、磷酸一氢钾、磷酸一氢钠、磷酸一氢铵、磷酸二氢钾、磷酸二氢钠、磷酸二氢铵中的至少两种的混合物；所用油类为可用于口腔护理的一切非极性物质包括但不仅限于油菜籽油、花生油、火麻油、玉米油、橄榄油、山茶油、棕榈油、大豆油、芝麻油、亚麻籽油(胡麻油)、葡萄籽油、核桃油、牡丹籽油、椰子油、食用石蜡、松节油、猪油、牛油、羊油、所有鱼类油脂、蛙油、蛇油、有机硅油、直链烷烃类、脂类、与水不互溶的醇类中的一种，或者油菜籽油、花生油、火麻油、玉米油、橄榄油、山茶油、棕榈油、葵花子油、大豆油、芝麻油、亚麻籽油(胡麻油)、葡萄籽油、核桃油、牡丹籽油、椰子油、食用石蜡、松节油、猪油、牛油、羊油、所有鱼类油脂、蛙油、蛇油、有机硅油、直链烷烃类、脂类、与水不互溶的醇类中的至少两种的混合油。
牙釉质再矿化试验表明，本实施例的牙釉质再矿化速率为普通含羟基磷灰石牙膏的23-83倍。
实施例5
1)制备固体粒子稳定的含有可溶性钙盐的水包油包水乳液：
将0.2克氧化锌加入50克橄榄油中，加热至30℃搅拌均匀制得油相。然后将2.5毫升2％的葡萄糖酸钙溶液和7.5毫升含有氧化锌的橄榄油加热至30℃进行混合，用高速分散机以6000转/分的速率分散40分钟，得到油包水乳液。
将2克磷酸钙加入25克水中，加热至30℃搅拌均匀制得水相。将3毫升制得的油包水乳液和2毫升水相加热至30℃进行混合，用高速分散机以4000转/分的速率分散20分钟，得到含有钙离子的水包油包水乳液。
2)制备固体粒子稳定的含有可溶性磷酸盐的水包油包水乳液：
将0.6克用硅烷偶联剂改性的碳酸钙加入10克花生油中，加热至30℃搅拌均匀制得油相。然后将2毫升5.5％的磷酸氢二钠溶液和5毫升含有改性羟基磷灰石的花生油加热至30℃进行混合，用高速分散机以18000转/分的速率分散10分钟，得到油包水乳液。
将1.2克氢氧化镁加入10克水中，制得水相。将3毫升制得的油包水乳液和5毫升水相加热至30℃进行混合，用高速分散机以5000转/分的速率分散40分钟，得到含有磷酸根离子的水包油包水乳液。
3)制备漱口水基质
用公知的方法制备含有保湿剂、表面活性剂、增稠剂、甜味剂、防腐剂、活性添加物、香料等组分的漱口水基质。
4)制备同时含有可溶性钙盐和可溶性磷酸盐的漱口水
将3克含有可溶性钙盐的水包油包水乳液和含有可溶性磷酸盐的水包油包水乳液以及3克漱口水基质加热至30℃进行混合，用高速分散机以9000转/分的速率分散15分钟，得到漱口水成品。这里说的含有可溶性钙盐的水包油包水乳液所含钙离子的物质的量与含有可溶性磷酸盐的水包油包水乳液所含磷酸根离子的物质的量之比为5：3。
牙釉质再矿化试验表明，本实施例的牙釉质再矿化速率为普通漱口水的24倍。
实施例6
1)制备固体粒子稳定的含有可溶性钙盐的水包油包水乳液：
将0.5克用十二烷基硫酸钠改性的二氧化钛加入椰子油中，加热至30℃搅拌均匀制得油相。然后将3.5毫升5％的碳酸氢钙溶液和3.5毫升含有改性二氧化钛的橄榄油加热至30℃进行混合，用高速分散机以7500转/分的速率分散15分钟，得到油包水乳液。
将2克硅藻土加入50克水中，制得水相。将2毫升制得的油包水乳液和2毫升水相加热至30℃进行混合，用高速分散机以15000转/分的速率分散20分钟，得到含有钙离子的水包油包水乳液。
2)制备固体粒子稳定的含有可溶性磷酸盐的水包油包水乳液：
将0.6克羟基磷灰石加入10克大豆油中，加热至30℃搅拌均匀制得油相。然后将1毫升3.6％的磷酸氢二氨溶液和4毫升含有羟基磷灰石的大豆油加热至30℃进行混合，用高速分散机以1200转/分的速率分散70分钟，得到油包水乳液。
将0.8克硅酸镁加入20克水中，搅拌均匀制得水相。将1.5毫升制得的油包水乳液和1毫升水相加热至30℃进行混合，用高速分散机以12000转/分的速率分散45分钟，得到含有磷酸根离子的水包油包水乳液。
3)制备漱口水基质
用公知的方法制备含有保湿剂、表面活性剂、增稠剂、甜味剂、防腐剂、活性添加物、香料等组分的漱口水基质。
4)制备同时含有可溶性钙盐和可溶性磷酸盐的牙膏
将3克含有钙离子的水包油包水乳液和含有磷酸根离子的水包油包水乳液以及2克漱口水基质加热至30℃进行混合，用高速分散机以8000转/分的速率搅拌35分钟，得到漱口水成品。这里说的含有可溶性钙盐的水包油包水乳液所含钙离子的物质的量与含有可溶性磷酸盐的水包油包水乳液所含磷酸根离子的物质的量之比为5：3。
牙釉质再矿化试验表明，本实施例的牙釉质再矿化速率为普通漱口水的17倍。
以上所述，仅是本发明的较佳实施例，并非对本发明作任何限制，凡是根据本发明技术实质对以上实施例所作的任何简单修改、变更以及等效结构变化，均仍属于本发明技术方案的保护范围内。
Claims (4)
1.一种牙釉质再生组合物的制备方法，其特征在于包括以下步骤：
1)制备固体粒子稳定的含有可溶性钙盐的水包油包水乳液：
将用于制备固体稳定乳液的选自有机或无机微纳米粒子或其混合物的固体粒子按0.1～25：100的质量比加入到用于口腔治疗的水剂或凝胶剂、或者制备牙膏、漱口水或者牙釉质修复凝胶用的植物来源、动物来源或矿物来源的天然油脂中、或者加入到以石油化工产品及天然提取原料加工的合成油脂中，加热至30℃～80℃，搅拌均匀形成油相a；
将能够溶解于水并能够产生游离态钙离子的物质加入水中，制成钙离子浓度为0.1％～60％的水溶液a，将所述水溶液a和上述油相a按0.5：9.5～1.5：0.5的体积比混合后置于高速分散机上加热至30℃～80℃，以10转/分至24000转/分搅拌0.5分钟～120分钟，得到油包水乳液a；
将用于制备固体稳定乳液的选自有机或无机微纳米粒子或其混合物的固体粒子按0.1～25：100的质量比加入水中，得到水相溶液a，将上述油包水乳液a与所述水相溶液a按0.5：9.5至1.5：0.5的体积比混合后置于高速分散机上加热至30℃～80℃，以10转/分至24000转/分搅拌0.5分钟～120分钟，得到含有可溶性钙盐的水包油包水乳液；
2)制备固体粒子稳定的含有可溶性磷酸盐的水包油包水乳液：
将用于制备固体稳定乳液的选自有机或无机微纳米粒子或其混合物的固体粒子按0.1～25：100的质量比加入到用于口腔治疗或者制备牙膏、漱口水或者牙釉质修复凝胶用的植物来源、动物来源或者矿物来源的天然油脂中，或者加入到以石油化工产品及天然提取原料加工的合成油脂中，加热至30℃～80℃，搅拌均匀形成油相b；
将能够提供游离态磷酸根、磷酸氢根或磷酸二氢根离子的化合物加入水中，制成磷酸根、磷酸氢根或磷酸二氢根离子浓度为0.1％～60％的水溶液b，将所述水溶液b和所述油相b按0.5：9.5～1.5：0.5的体积比混合后置于高速分散机上，加热至30℃～80℃，以10转/分至24000转/分搅拌0.5分钟～120分钟，得到油包水乳液b；
将用于制备固体稳定乳液的选自有机或无机微纳米粒子或其混合物的固体粒子按0.1～25：100的质量比加入水中，得到水相溶液b，将所述油包水乳液b与所述水相溶液b按0.5：9.5至1.5：0.5的体积比混合后置于高速分散机上加热至30℃～80℃，以10转/分至24000转/分搅拌0.5分钟～120分钟，得到含有可溶性磷酸盐的水包油包水乳液；
所述步骤1、2)的固体粒子为二氧化硅、三氧化二铝、生物活性玻璃、碳酸钙、硅酸钙、磷酸钙、羟基磷灰石、氧化锌、二氧化钛、碳酸镁、氢氧化镁、硅藻土、蒙脱土、水滑石、云母、凹凸棒、沸石、聚乙烯、聚苯乙烯、聚丙烯酸类树脂、天然植物粉末及其表面改性的天然植物粉末、纤维素及其官能团两亲化衍生物中的一种或者至少两种的混合粒子；
所述步骤1、2)的天然油脂或合成油脂为菜籽油、花生油、玉米油、橄榄油、山茶油、棕榈油、葵花子油、大豆油、芝麻油、亚麻籽油、葡萄籽油、核桃油、牡丹籽油、椰子油，食用石蜡、松节油、猪油、牛油、羊油、鱼类油脂、蛙油、蛇油、有机硅油中的一种或者至少两种的混合油；3)同时含有可溶性钙盐和可溶性磷酸盐的漱口水、牙膏或牙釉质修复凝胶的制备步骤如下：
将加热至30℃～80℃的含有可溶性钙盐的水包油包水乳液、含有可溶性磷酸盐的水包油包水乳液和漱口水基质、牙膏基质或牙釉质修复凝胶基质混合，以10转/分至24000转/分搅拌0.5分钟～120分钟，得到同时含有可溶性钙盐和可溶性磷酸盐的漱口水、牙膏或牙釉质修复凝胶，即得到所述牙釉质再生组合物；其中，含有可溶性钙盐的水包油包水乳液所含的钙离子的量与含有可溶性磷酸盐的水包油包水乳液所含磷酸根离子的量的比为5：3，含有可溶性钙盐的水包油包水乳液和含有可溶性磷酸盐的水包油包水乳液的总量与漱口水基质、牙膏基质或牙釉质修复凝胶基质的量的质量比为1：19至19：1。
2.根据权利要求1所述的牙釉质再生组合物的制备方法，其特征在于：所述步骤1、2)的固体粒子用以下物质替代：经过用硅烷偶联剂、钛酸酯偶联剂或表面活性剂进行改性的二氧化硅、三氧化二铝、生物活性玻璃、碳酸钙、硅酸钙、磷酸钙、羟基磷灰石、氧化锌、二氧化钛、碳酸镁、氢氧化镁、硅藻土、蒙脱土、水滑石、云母、凹凸棒和沸石中的一种或者至少两种的混合粒子；
用于改性固体粒子的表面活性剂为用于口腔清洁护理用品的十二烷基硫酸钠、十二烷基苯磺酸钠、葡聚糖苷类非离子表面活性剂、甜菜碱中的一种或者至少两种的混合物。
3.根据权利要求1或2所述的牙釉质再生组合物的制备方法，其特征在于：所述的能够产生游离态钙离子的物质为氯化钙、氢氧化钙、氧化钙、硝酸钙、葡萄糖酸钙、碳酸氢钙、乳酸钙中的一种或者至少两种的混合物。
4.根据权利要求1或2所述的牙釉质再生组合物的制备方法，其特征在于：所述的能够产生游离态磷酸根、磷酸氢根或磷酸二氢根离子的化合物，选自磷酸钾、磷酸钠、磷酸铵、磷酸一氢钾、磷酸一氢钠、磷酸一氢铵、磷酸二氢钾、磷酸二氢钠、磷酸二氢铵中的一种或者至少两种的混合物。
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