WO2022264811A1 - Dentifrice composition - Google Patents
Dentifrice composition Download PDFInfo
- Publication number
- WO2022264811A1 WO2022264811A1 PCT/JP2022/022269 JP2022022269W WO2022264811A1 WO 2022264811 A1 WO2022264811 A1 WO 2022264811A1 JP 2022022269 W JP2022022269 W JP 2022022269W WO 2022264811 A1 WO2022264811 A1 WO 2022264811A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- fluorine
- dentifrice composition
- fluoride
- component
- retention
- Prior art date
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 72
- 239000000551 dentifrice Substances 0.000 title claims abstract description 45
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 46
- 239000011737 fluorine Substances 0.000 claims abstract description 46
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229920002678 cellulose Polymers 0.000 claims abstract description 18
- 239000001913 cellulose Substances 0.000 claims abstract description 18
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- 239000001736 Calcium glycerylphosphate Substances 0.000 claims abstract description 12
- UHHRFSOMMCWGSO-UHFFFAOYSA-L calcium glycerophosphate Chemical compound [Ca+2].OCC(CO)OP([O-])([O-])=O UHHRFSOMMCWGSO-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229940095618 calcium glycerophosphate Drugs 0.000 claims abstract description 12
- 235000019299 calcium glycerylphosphate Nutrition 0.000 claims abstract description 12
- 229920000388 Polyphosphate Polymers 0.000 claims abstract description 9
- 239000001205 polyphosphate Substances 0.000 claims abstract description 9
- 235000011176 polyphosphates Nutrition 0.000 claims abstract description 9
- -1 fluorine ions Chemical class 0.000 claims description 61
- 229940034610 toothpaste Drugs 0.000 claims description 10
- 239000000606 toothpaste Substances 0.000 claims description 10
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 claims description 5
- 230000014759 maintenance of location Effects 0.000 abstract description 38
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract description 37
- 239000007788 liquid Substances 0.000 abstract description 25
- 238000000926 separation method Methods 0.000 abstract description 25
- 210000002200 mouth mucosa Anatomy 0.000 abstract description 11
- 238000003860 storage Methods 0.000 abstract description 11
- 229940091249 fluoride supplement Drugs 0.000 description 30
- 210000000214 mouth Anatomy 0.000 description 22
- 238000007711 solidification Methods 0.000 description 21
- 230000008023 solidification Effects 0.000 description 21
- 230000000694 effects Effects 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 13
- 238000011156 evaluation Methods 0.000 description 13
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 12
- 239000000796 flavoring agent Substances 0.000 description 10
- 235000019634 flavors Nutrition 0.000 description 10
- 238000009472 formulation Methods 0.000 description 10
- 239000003921 oil Substances 0.000 description 10
- 235000019198 oils Nutrition 0.000 description 10
- 239000011230 binding agent Substances 0.000 description 9
- 230000000717 retained effect Effects 0.000 description 9
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 8
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 8
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 239000002304 perfume Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 235000014113 dietary fatty acids Nutrition 0.000 description 6
- 239000000194 fatty acid Substances 0.000 description 6
- 229930195729 fatty acid Natural products 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 239000011775 sodium fluoride Substances 0.000 description 6
- 235000013024 sodium fluoride Nutrition 0.000 description 6
- 239000003082 abrasive agent Substances 0.000 description 5
- 229910001634 calcium fluoride Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005227 gel permeation chromatography Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 210000003296 saliva Anatomy 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 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 4
- 239000002202 Polyethylene glycol Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 3
- 235000013162 Cocos nucifera Nutrition 0.000 description 3
- 244000060011 Cocos nucifera Species 0.000 description 3
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000004480 active ingredient Substances 0.000 description 3
- 230000001680 brushing effect Effects 0.000 description 3
- 229910001424 calcium ion Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 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
- 208000002925 dental caries Diseases 0.000 description 3
- YIOJGTBNHQAVBO-UHFFFAOYSA-N dimethyl-bis(prop-2-enyl)azanium Chemical class C=CC[N+](C)(C)CC=C YIOJGTBNHQAVBO-UHFFFAOYSA-N 0.000 description 3
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 description 3
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- OSWPMRLSEDHDFF-UHFFFAOYSA-N methyl salicylate Chemical compound COC(=O)C1=CC=CC=C1O OSWPMRLSEDHDFF-UHFFFAOYSA-N 0.000 description 3
- 239000008213 purified water Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 238000013268 sustained release Methods 0.000 description 3
- 239000012730 sustained-release form Substances 0.000 description 3
- 230000008719 thickening Effects 0.000 description 3
- XHXUANMFYXWVNG-ADEWGFFLSA-N (-)-Menthyl acetate Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@H]1OC(C)=O XHXUANMFYXWVNG-ADEWGFFLSA-N 0.000 description 2
- CFAKWWQIUFSQFU-UHFFFAOYSA-N 2-hydroxy-3-methylcyclopent-2-en-1-one Chemical compound CC1=C(O)C(=O)CC1 CFAKWWQIUFSQFU-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QFOHBWFCKVYLES-UHFFFAOYSA-N Butylparaben Chemical compound CCCCOC(=O)C1=CC=C(O)C=C1 QFOHBWFCKVYLES-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- VTAJIXDZFCRWBR-UHFFFAOYSA-N Licoricesaponin B2 Natural products C1C(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2)C(O)=O)C)(C)CC2)(C)C2C(C)(C)CC1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O VTAJIXDZFCRWBR-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 235000011203 Origanum Nutrition 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000002280 amphoteric surfactant Substances 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- CUFNKYGDVFVPHO-UHFFFAOYSA-N azulene Chemical compound C1=CC=CC2=CC=CC2=C1 CUFNKYGDVFVPHO-UHFFFAOYSA-N 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- FUWUEFKEXZQKKA-UHFFFAOYSA-N beta-thujaplicin Chemical compound CC(C)C=1C=CC=C(O)C(=O)C=1 FUWUEFKEXZQKKA-UHFFFAOYSA-N 0.000 description 2
- 229960003237 betaine Drugs 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 235000010418 carrageenan Nutrition 0.000 description 2
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- 229940113118 carrageenan Drugs 0.000 description 2
- ULDHMXUKGWMISQ-UHFFFAOYSA-N carvone Chemical compound CC(=C)C1CC=C(C)C(=O)C1 ULDHMXUKGWMISQ-UHFFFAOYSA-N 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000005115 demineralization Methods 0.000 description 2
- 230000002328 demineralizing effect Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 235000011180 diphosphates Nutrition 0.000 description 2
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 description 2
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 description 2
- 235000003599 food sweetener Nutrition 0.000 description 2
- 239000013022 formulation composition Substances 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 239000008369 fruit flavor Substances 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- LPLVUJXQOOQHMX-UHFFFAOYSA-N glycyrrhetinic acid glycoside Natural products C1CC(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2=O)C(O)=O)C)(C)CC2)(C)C2C(C)(C)C1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O LPLVUJXQOOQHMX-UHFFFAOYSA-N 0.000 description 2
- 239000001685 glycyrrhizic acid Substances 0.000 description 2
- UYRUBYNTXSDKQT-UHFFFAOYSA-N glycyrrhizic acid Natural products CC1(C)C(CCC2(C)C1CCC3(C)C2C(=O)C=C4C5CC(C)(CCC5(C)CCC34C)C(=O)O)OC6OC(C(O)C(O)C6OC7OC(O)C(O)C(O)C7C(=O)O)C(=O)O UYRUBYNTXSDKQT-UHFFFAOYSA-N 0.000 description 2
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- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 description 2
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- FOYKKGHVWRFIBD-UHFFFAOYSA-N gamma-tocopherol acetate Natural products CC(=O)OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1 FOYKKGHVWRFIBD-UHFFFAOYSA-N 0.000 description 1
- WTEVQBCEXWBHNA-JXMROGBWSA-N geranial Chemical compound CC(C)=CCC\C(C)=C\C=O WTEVQBCEXWBHNA-JXMROGBWSA-N 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000010651 grapefruit oil Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 235000001050 hortel pimenta Nutrition 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 description 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 1
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 1
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 1
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 1
- 239000012729 immediate-release (IR) formulation Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- NFIDBGJMFKNGGQ-UHFFFAOYSA-N isopropylmethylphenol Natural products CC(C)CC1=CC=CC=C1O NFIDBGJMFKNGGQ-UHFFFAOYSA-N 0.000 description 1
- 239000010656 jasmine oil Substances 0.000 description 1
- 235000010494 karaya gum Nutrition 0.000 description 1
- 239000000231 karaya gum Substances 0.000 description 1
- 229940039371 karaya gum Drugs 0.000 description 1
- VQHSOMBJVWLPSR-JVCRWLNRSA-N lactitol Chemical compound OC[C@H](O)[C@@H](O)[C@@H]([C@H](O)CO)O[C@@H]1O[C@H](CO)[C@H](O)[C@H](O)[C@H]1O VQHSOMBJVWLPSR-JVCRWLNRSA-N 0.000 description 1
- 229940094522 laponite Drugs 0.000 description 1
- 239000000171 lavandula angustifolia l. flower oil Substances 0.000 description 1
- 239000010501 lemon oil Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 229940087305 limonene Drugs 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- 229930007744 linalool Natural products 0.000 description 1
- UWKAYLJWKGQEPM-UHFFFAOYSA-N linalool acetate Natural products CC(C)=CCCC(C)(C=C)OC(C)=O UWKAYLJWKGQEPM-UHFFFAOYSA-N 0.000 description 1
- 229920000092 linear low density polyethylene Polymers 0.000 description 1
- 239000004707 linear low-density polyethylene Substances 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- XCOBTUNSZUJCDH-UHFFFAOYSA-B lithium magnesium sodium silicate Chemical compound [Li+].[Li+].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Na+].[Na+].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3.O1[Si](O2)([O-])O[Si]3([O-])O[Si]1([O-])O[Si]2([O-])O3 XCOBTUNSZUJCDH-UHFFFAOYSA-B 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- 239000004325 lysozyme Substances 0.000 description 1
- 235000010335 lysozyme Nutrition 0.000 description 1
- 229960000274 lysozyme Drugs 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 229910000400 magnesium phosphate tribasic Inorganic materials 0.000 description 1
- VQHSOMBJVWLPSR-WUJBLJFYSA-N maltitol Chemical compound OC[C@H](O)[C@@H](O)[C@@H]([C@H](O)CO)O[C@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O VQHSOMBJVWLPSR-WUJBLJFYSA-N 0.000 description 1
- 239000001683 mentha spicata herb oil Substances 0.000 description 1
- 229940041616 menthol Drugs 0.000 description 1
- 229930007503 menthone Natural products 0.000 description 1
- 229940102398 methyl anthranilate Drugs 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000004292 methyl p-hydroxybenzoate Substances 0.000 description 1
- 235000010270 methyl p-hydroxybenzoate Nutrition 0.000 description 1
- 229960001047 methyl salicylate Drugs 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 229960002216 methylparaben Drugs 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 235000019796 monopotassium phosphate Nutrition 0.000 description 1
- DVEKCXOJTLDBFE-UHFFFAOYSA-N n-dodecyl-n,n-dimethylglycinate Chemical compound CCCCCCCCCCCC[N+](C)(C)CC([O-])=O DVEKCXOJTLDBFE-UHFFFAOYSA-N 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- ITVGXXMINPYUHD-CUVHLRMHSA-N neohesperidin dihydrochalcone Chemical compound C1=C(O)C(OC)=CC=C1CCC(=O)C(C(=C1)O)=C(O)C=C1O[C@H]1[C@H](O[C@H]2[C@@H]([C@H](O)[C@@H](O)[C@H](C)O2)O)[C@@H](O)[C@H](O)[C@@H](CO)O1 ITVGXXMINPYUHD-CUVHLRMHSA-N 0.000 description 1
- 229940089953 neohesperidin dihydrochalcone Drugs 0.000 description 1
- 235000010434 neohesperidine DC Nutrition 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000010502 orange oil Substances 0.000 description 1
- 229930007459 p-menth-8-en-3-one Natural products 0.000 description 1
- 229940070802 palmitoyl glutamate Drugs 0.000 description 1
- RUVINXPYWBROJD-UHFFFAOYSA-N para-methoxyphenyl Natural products COC1=CC=C(C=CC)C=C1 RUVINXPYWBROJD-UHFFFAOYSA-N 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000223 polyglycerol Polymers 0.000 description 1
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 description 1
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000001508 potassium citrate Substances 0.000 description 1
- 229960002635 potassium citrate Drugs 0.000 description 1
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 1
- 235000011082 potassium citrates Nutrition 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- HELXLJCILKEWJH-NCGAPWICSA-N rebaudioside A Chemical compound O([C@H]1[C@H](O)[C@@H](CO)O[C@H]([C@@H]1O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)O[C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O HELXLJCILKEWJH-NCGAPWICSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000003578 releasing effect Effects 0.000 description 1
- 230000000395 remineralizing effect Effects 0.000 description 1
- 239000010666 rose oil Substances 0.000 description 1
- 235000019719 rose oil Nutrition 0.000 description 1
- 239000010668 rosemary oil Substances 0.000 description 1
- 229940058206 rosemary oil Drugs 0.000 description 1
- 239000010670 sage oil Substances 0.000 description 1
- 108700004121 sarkosyl Proteins 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 229940079841 sodium copper chlorophyllin Drugs 0.000 description 1
- 235000013758 sodium copper chlorophyllin Nutrition 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- KSAVQLQVUXSOCR-UHFFFAOYSA-M sodium lauroyl sarcosinate Chemical compound [Na+].CCCCCCCCCCCC(=O)N(C)CC([O-])=O KSAVQLQVUXSOCR-UHFFFAOYSA-M 0.000 description 1
- 229940045885 sodium lauroyl sarcosinate Drugs 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- AQMNWCRSESPIJM-UHFFFAOYSA-M sodium metaphosphate Chemical compound [Na+].[O-]P(=O)=O AQMNWCRSESPIJM-UHFFFAOYSA-M 0.000 description 1
- 229960004711 sodium monofluorophosphate Drugs 0.000 description 1
- 229940060304 sodium myristoyl sarcosinate Drugs 0.000 description 1
- 229950005425 sodium myristyl sulfate Drugs 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- KHCOJQDJOCNUGV-UHFFFAOYSA-M sodium;2-[methyl(tetradecanoyl)amino]acetate Chemical compound [Na+].CCCCCCCCCCCCCC(=O)N(C)CC([O-])=O KHCOJQDJOCNUGV-UHFFFAOYSA-M 0.000 description 1
- SMKZBQZAMSKHNS-UHFFFAOYSA-M sodium;2-sulfoacetate Chemical compound [Na+].OS(=O)(=O)CC([O-])=O SMKZBQZAMSKHNS-UHFFFAOYSA-M 0.000 description 1
- UPUIQOIQVMNQAP-UHFFFAOYSA-M sodium;tetradecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCOS([O-])(=O)=O UPUIQOIQVMNQAP-UHFFFAOYSA-M 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 235000019721 spearmint oil Nutrition 0.000 description 1
- OHHNJQXIOPOJSC-UHFFFAOYSA-N stevioside Natural products CC1(CCCC2(C)C3(C)CCC4(CC3(CCC12C)CC4=C)OC5OC(CO)C(O)C(O)C5OC6OC(CO)C(O)C(O)C6O)C(=O)OC7OC(CO)C(O)C(O)C7O OHHNJQXIOPOJSC-UHFFFAOYSA-N 0.000 description 1
- 229940013618 stevioside Drugs 0.000 description 1
- 235000019202 steviosides Nutrition 0.000 description 1
- 229910001631 strontium chloride Inorganic materials 0.000 description 1
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229960003080 taurine Drugs 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- GBNXLQPMFAUCOI-UHFFFAOYSA-H tetracalcium;oxygen(2-);diphosphate Chemical compound [O-2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GBNXLQPMFAUCOI-UHFFFAOYSA-H 0.000 description 1
- 239000010678 thyme oil Substances 0.000 description 1
- 229960000790 thymol Drugs 0.000 description 1
- YUOWTJMRMWQJDA-UHFFFAOYSA-J tin(iv) fluoride Chemical compound [F-].[F-].[F-].[F-].[Sn+4] YUOWTJMRMWQJDA-UHFFFAOYSA-J 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- GYDJEQRTZSCIOI-LJGSYFOKSA-N tranexamic acid Chemical compound NC[C@H]1CC[C@H](C(O)=O)CC1 GYDJEQRTZSCIOI-LJGSYFOKSA-N 0.000 description 1
- 229960000401 tranexamic acid Drugs 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical class [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 229960003500 triclosan Drugs 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 1
- VXYADVIJALMOEQ-UHFFFAOYSA-K tris(lactato)aluminium Chemical compound CC(O)C(=O)O[Al](OC(=O)C(C)O)OC(=O)C(C)O VXYADVIJALMOEQ-UHFFFAOYSA-K 0.000 description 1
- UJMBCXLDXJUMFB-UHFFFAOYSA-K trisodium;5-oxo-1-(4-sulfonatophenyl)-4-[(4-sulfonatophenyl)diazenyl]-4h-pyrazole-3-carboxylate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)C1=NN(C=2C=CC(=CC=2)S([O-])(=O)=O)C(=O)C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 UJMBCXLDXJUMFB-UHFFFAOYSA-K 0.000 description 1
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 description 1
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 description 1
- 235000012141 vanillin Nutrition 0.000 description 1
- 239000009637 wintergreen oil Substances 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
- 229930007845 β-thujaplicin Natural products 0.000 description 1
Classifications
-
- 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/55—Phosphorus 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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
-
- 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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/731—Cellulose; Quaternized cellulose derivatives
-
- 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
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/54—Polymers characterized by specific structures/properties
- A61K2800/542—Polymers characterized by specific structures/properties characterized by the charge
- A61K2800/5426—Polymers characterized by specific structures/properties characterized by the charge cationic
Definitions
- the present invention relates to a dentifrice composition containing a water-soluble fluorine-containing compound that is excellent in retention of fluoride ions in the oral cavity, particularly in the oral mucosa, and also excellent in release.
- Fluorine-containing compounds such as sodium fluoride are widely used in oral compositions such as dentifrice compositions for the purpose of preventing dental caries as medicinal ingredients having functions such as promoting remineralization and inhibiting demineralization. .
- it is effective to allow the fluorine ions to remain on the tooth surface in the oral cavity for a long period of time. Although it is important to retain a large amount of fluoride ions in the oral cavity even afterward, only a very small amount of fluoride ions remained in the oral cavity because the dentifrice composition was washed away by rinsing after brushing.
- Patent Document 2 Japanese Patent Application Laid-Open No. 2009-137863 proposes a composition in which a complex of a polyphosphate, a calcium salt, and a fluoride salt is prepared in advance. There were problems such as liquefaction and solidification after long-term storage as a dentifrice preparation.
- Patent Documents 3 to 5 JP-A-2015-117215, JP-A-2013-67567, JP-A-2007-320894) disclose that a specific cationic polymeric substance is used in a dentifrice composition. However, there is still room for improvement in retention and the amount remaining after brushing, and further improvement in retention has been desired.
- the present invention has been made in view of the above circumstances, and an object thereof is to provide a dentifrice composition which is excellent in retention of fluoride ions in the oral cavity, particularly in the oral mucosa, and which is also excellent in releasability.
- a dentifrice composition comprising a water-soluble fluorine-containing compound, a water-soluble polyphosphate and calcium glycerophosphate, and a cationized cellulose.
- a dentifrice composition comprising a water-soluble fluorine-containing compound, a water-soluble polyphosphate and calcium glycerophosphate, and a cationized cellulose.
- a dentifrice composition containing (A) a water-soluble polyphosphate, (B) calcium glycerophosphate, (C) a water-soluble fluorine-containing compound, and (D) a cationized cellulose is used in the oral cavity, particularly
- the inventors have found that the fluorine ion retains well in the oral mucosa, is excellent in its releasability, has good liquid separation stability, solidification stability, and good storage stability, and has completed the present invention.
- the fluorine contained in the water-soluble fluorine-containing compound contained in the dentifrice composition sufficiently retained not only on the tooth surface but also on the oral mucosa, the retention in the oral cavity would be further enhanced. Since it is covered with salivary proteins, it is difficult for fluorine to be adsorbed.
- the components (A) and (B) are used in combination with the component (C), and the component (D) is combined. As a result, not only the retention of fluorine ions but also the releasability of fluorine ions was improved.
- the component (D) enhances the adsorption of fluoride ions to the mucin covering the oral mucosa, thereby improving its retention, and the fluoride ions stay in the oral mucosa at a high rate and stay. Fluoride ions are gradually released into saliva and supplied to the tooth surface in contact with saliva for a long period of time. Therefore, according to the dentifrice composition of the present invention, the liquid separation stability and the solidification stability can be ensured, and the retention of fluoride ions in the oral cavity can be improved.
- the dentifrice compositions containing the components (A), (B), (C) and (D) of the present invention are excellent in fluorine retention and fluorine release.
- the liquid separation stability and solidification stability of the formulation were good.
- the present invention provides the following dentifrice composition.
- A a water-soluble polyphosphate
- B calcium glycerophosphate
- A The dentifrice composition according to [1], wherein the component is potassium pyrophosphate.
- A The dentifrice composition according to [1] or [2], wherein (A)/(C) has a molar ratio of 0.05 to 1.
- A The dentifrice composition according to any one of [1] to [3], wherein (B)/(C) is 0.05 to 1.5 as a molar ratio.
- the content of component (A) is 0.1 to 1.5% by mass
- the content of component (B) is 0.1 to 2% by mass
- the content of component (C) is 500 to 5,000 ppm as fluorine ions.
- a dentifrice composition is excellent in retention of fluorine ions in the oral cavity, particularly in the oral mucosa, is also excellent in its releasability, and has good liquid separation stability, solidification stability, and storage stability. can provide things.
- the dentifrice composition of the present invention can retain a relatively large amount of fluoride ions in the oral cavity even after gargling and rinsing the oral cavity after brushing, and remineralization of the water-soluble fluorine-containing compound. It is also suitable for caries prevention because it can sufficiently exhibit effects such as acceleration of caries and inhibition of demineralization.
- the dentifrice composition of the present invention contains (A) a water-soluble polyphosphate, (B) calcium glycerophosphate, (C) a water-soluble fluorine-containing compound, and (D) cationized cellulose.
- the water-soluble polyphosphate has an effect of improving retention of fluorine ions and an effect of suppressing liquid separation.
- the water-soluble polyphosphate includes linear polyphosphoric acids such as pyrophosphoric acid, tripolyphosphoric acid and tetrapolyphosphoric acid, and cyclic polyphosphoric acids such as trimetaphosphoric acid, tetrametaphosphoric acid and hexametaphosphoric acid.
- the salts thereof include alkali metal salts such as sodium salts and potassium salts. Among them, pyrophosphate and tripolyphosphate are preferred, pyrophosphate is more preferred, and potassium pyrophosphate is particularly preferred. These may be used singly or in combination of two or more.
- the amount of component (A) is preferably 0.1 to 1.5% (mass%, hereinafter the same) of the entire composition, more preferably 0.15 to 1.4%, and still more preferably 0.3 to 1.0%.
- the blending amount is 0.1% or more, sufficient retention and release of fluorine ions can be obtained, and liquid separation can be suppressed over time to obtain sufficient liquid separation stability.
- the content is 1.5% or less, retention and release properties of fluoride ions are sufficiently maintained, and solidification over time is prevented to obtain sufficient solidification stability.
- Calcium glycerophosphate has an effect of improving retention of fluorine ions and an effect of suppressing solidification.
- Calcium glycerophosphate may be derived from natural products or synthetic products.
- a commercially available product such as “calcium glycerophosphate” manufactured by Iwaki Seiyaku Co., Ltd. can also be used.
- the content of calcium glycerophosphate is preferably 0.1 to 2%, more preferably 0.15 to 1.8%, and particularly preferably 0.25 to 1.5% of the total composition.
- the blending amount is 0.1% or more, sufficient retention and release of fluorine ions can be obtained, and solidification over time can be prevented to obtain sufficient solidification stability.
- the content is 2% or less, the retention and release properties of fluoride ions are sufficiently maintained, and liquid separation over time is suppressed to obtain sufficient liquid separation stability.
- Water-soluble fluorine-containing compounds include sodium fluoride, sodium monofluorophosphate, tin fluoride and the like.
- the content of the water-soluble fluorine-containing compound is preferably 500 to 5,000 ppm, more preferably 1,100 to 3,000 ppm, in terms of fluorine ions, based on the total composition. When the content is 500 ppm or more in terms of fluoride ions, the retention effect of fluoride ions is sufficiently improved, and when it is 5,000 ppm or less, adverse effects such as mottled teeth due to excessive intake can be prevented.
- the blending amount of the water-soluble fluorine-containing compound varies depending on the amount of fluoride ions to be supplied.
- the amount to be blended is 0.11% of the total composition.
- the content of sodium fluoride is preferably 0.1% or more, more preferably 0.25 to 0.7%, based on the total composition.
- (A)/(C), which indicates the quantitative ratio of component (A) and component (C) is preferably 0.05 to 1, more preferably 0.1 to 0.5, as a molar ratio. In particular, it is 0.10 to 0.50.
- (B)/(C), which indicates the quantitative ratio of component (B) to component (C) is preferably 0.05 to 1.5, more preferably 0.10 to 1 as a molar ratio. More preferably, the molar ratio of (A)/(C) and the molar ratio of (B)/(C) are within the above ranges. When the component (C) is blended within these molar ratio ranges, the retention and release properties of fluorine ions are more excellent, and the liquid separation stability and solidification stability are more excellent.
- Cationized cellulose is cellulose with cations or cellulose derivatives with cations.
- the cationized cellulose may have counterions (eg, halogen ions (chloride ions), methosulfate ions, etc.).
- the molecular weight of cationized cellulose is not particularly limited.
- the component (D) one type of cationized cellulose may be used alone, or two or more types may be used in combination.
- Examples of cationized cellulose include hydroxyethylcellulose dimethyldiallylammonium salt, O-[2-hydroxy-3-(trimethylammonio)propyl]hydroxyethylcellulose chloride, preferably hydroxyethylcellulose dimethyldiallylammonium salt.
- Hydroxyethylcellulose dimethyldiallylammonium salt includes chloride ion as a counter ion, and hydroxyethylcellulose dimethyldiallylammonium chloride is preferable.
- the cationized cellulose used in the present invention has a 2% aqueous solution viscosity (BH type Brookfield viscometer, rotor No. 2, 20 rotations, 20°C, measurement time 1 minute) of 30 to 3,000 mPa s. preferable.
- the average molecular weight of the cationized cellulose is not particularly limited, it is preferably 100,000 to 1,500,000 as a weight-average molecular weight determined by gel permeation chromatography (GPC) using polyethylene glycol as a standard substance.
- the nitrogen content is preferably 0.1-3%, more preferably 0.5-2.5%.
- cationized cellulose examples include CELQUAT L-200 (2% aqueous solution viscosity: 35 to 350 mPa s, BH type Brookfield viscometer, rotor No. 2, 20 rotation, 20° C., measurement time of 1 minute), weight average molecular weight by gel permeation chromatography (GPC) method using polyethylene glycol as a standard substance: 250,000 to 350,000).
- the blending amount of component (D) is preferably 0.01-0.5%, more preferably 0.05-0.2% of the total composition.
- the content is 0.01% or more, sufficient retention and release of fluorine ions can be obtained, and liquid separation can be suppressed over time to obtain sufficient liquid separation stability. If it is 0.5% or less, discomfort to the oral mucosa is sufficiently suppressed.
- (A)/(D), which indicates the quantitative ratio of component (A) and component (D), is preferably 1-50, more preferably 3-25 as a mass ratio.
- (B)/(D), which indicates the quantitative ratio of component (B) to component (D), is preferably 1-50, more preferably 2-30 as a mass ratio.
- (C)/(D), which indicates the quantitative ratio between component (C) and component (D), is preferably 1-20, more preferably 1-10 as a mass ratio.
- the dentifrice composition of the present invention is particularly suitable as a toothpaste or gel-like dentifrice (abrasive-free), especially as a toothpaste, and in addition to the above ingredients, other known ingredients of the present invention It can be blended according to need within a range that does not interfere with the effect.
- abrasives, binders, thickeners, surfactants, and if necessary, colorants, sweeteners, preservatives, fragrances, active ingredients, etc. can be added.
- the method for preparing the dentifrice composition is not particularly limited, and may be a known method according to the dosage form. and can be prepared.
- abrasives examples include silica-based abrasives such as anhydrous silicic acid, precipitated silica, silica gel, aluminosilicate, and zirconosilicate; Calcium phosphate compounds such as tetracalcium phosphate and calcium pyrophosphate, calcium carbonate, calcium hydroxide, aluminum hydroxide, insoluble sodium metaphosphate, trimagnesium phosphate, magnesium carbonate, calcium sulfate, bentonite, titanium-bound silicate, synthetic resin Abrasives can be mentioned. Among them, silica-based abrasives are preferred. The compounding amount of the abrasive is preferably 5 to 60%, particularly 5 to 30% of the total composition.
- the binder can be an organic or inorganic binder.
- cellulose derivatives such as sodium carboxymethylcellulose, methylcellulose, hydroxymethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose, hydroxymethylethylcellulose, alginic acid derivatives such as sodium alginate, xanthan gum, tragacanth gum, karaya gum, gum arabic, etc.
- organic binders such as gums, polyacrylates, carrageenan, polyvinyl alcohol and carboxyvinyl polymer
- inorganic binders such as thickening silica, thickening aluminum silica, veegum and laponite.
- the content of the binder is preferably 0.1 to 5%, particularly 0.2 to 3%, of the total composition.
- an organic binder is particularly preferred, and the amount of the organic binder to be blended is preferably 0.1 to 5%, particularly 0.5 to 3%, of the total composition.
- the inorganic binder, especially the thickening silica is preferably 5% or less, particularly 2% or less, particularly preferably 1% or less of the total composition in terms of retention of fluorine ions, and even if it is not blended, it is 0%. good.
- Viscosity agents include sugar alcohols such as sorbit, xylit, erythritol, maltit and lactit, polyhydric alcohols such as glycerin, propylene glycol, and polyethylene glycol with an average molecular weight of 160 to 400 (average molecular weight according to the Standards for Quasi-drug Ingredients 2006). is mentioned.
- the blending amount of the thickening agent is usually 5 to 60% of the total composition.
- Surfactants can be blended with anionic surfactants, nonionic surfactants, and amphoteric surfactants.
- Anionic surfactants include alkyl sulfates such as sodium lauryl sulfate and sodium myristyl sulfate, acyl sarcosinates such as sodium lauroyl sarcosinate and sodium myristoyl sarcosinate, sodium dodecylbenzene sulfonate, hydrogenated coconut fatty acid monoglyceride monosodium sulfate, lauryl Examples include sodium sulfoacetate, acylglutamates such as sodium N-palmitoyl glutamate, sodium N-methyl-N-acyl taurine, sodium N-methyl-N-acylalanine, and sodium ⁇ -olefin sulfonate.
- Nonionic surfactants include polyoxyethylene alkyl ethers (for example, alkyl groups having 16 to 18 carbon atoms), polyoxyethylene hydrogenated castor oils (for example, those having an average added mole number of ethylene oxide of 40 to 80), Alkyl glucoside, polyoxyethylene polyoxypropylene block copolymer, polyglycerol fatty acid ester, sorbitan fatty acid ester, sucrose fatty acid ester, alkylolamide, polyoxyethylene sorbitan monostearate, polyoxyethylene polyoxypropylene glycol, etc. be done.
- polyoxyethylene alkyl ethers for example, alkyl groups having 16 to 18 carbon atoms
- polyoxyethylene hydrogenated castor oils for example, those having an average added mole number of ethylene oxide of 40 to 80
- Alkyl glucoside polyoxyethylene polyoxypropylene block copolymer
- polyglycerol fatty acid ester sorbitan fatty acid ester
- Amphoteric surfactants include betaine lauryldimethylaminoacetate, N-coconut fatty acid acyl-N-carboxymethyl-N-hydroxyethylethylenediamine, betaine coconut amidopropyldimethylaminoacetate, and amidopropyl coconut oil.
- the amount of the surfactant to be blended is usually 0.1 to 10% of the total composition. The blending amount can be adjusted depending on the form of the dentifrice composition, the purpose of use, etc. For example, 0.1 to 10% can be blended in a toothpaste.
- Colorants include Red No. 2, Red No. 3, Red No. 225, Red No. 226, Yellow No. 4, Yellow No. 5, Yellow No. 205, Blue No. 1, Blue No. 2, Blue No. 201, Blue No. 204, Green 3. No. 2, mica titanium, titanium oxide, and the like.
- Sweeteners include sodium saccharin, aspartame, stevioside, stevia extract, paramethoxycinnamic aldehyde, neohesperidin dihydrochalcone, perillartine and the like.
- the antiseptic include paraoxybenzoic acid esters such as methylparaben, ethylparaben and butylparaben, and benzoic acid such as sodium benzoate and salts thereof.
- Peppermint oil spearmint oil, anise oil, eucalyptus oil, wintergreen oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil, lime.
- the blending amount is not particularly limited, it is preferable to use 0.000001 to 1% of the above perfume material in the formulation composition. In addition, it is preferable to use 0.05 to 2% in the formulation composition as a perfume for perfume using the above perfume material.
- Active ingredients include bactericides such as isopropylmethylphenol and cetylpyridinium chloride, water-soluble phosphoric acid compounds such as orthophosphate potassium salts and sodium salts, enzymes such as dextranase, mutanase, amylase and protease, tranexamic acid, Epsilon aminocaproic acid, triclosan, lysozyme chloride, aluminum chlorohydroxyallantoin, hinokitiol, ascorbic acid, tocopheryl acetate, dihydrocholesterol, ⁇ -bisabolol, chlorhexidine salts, azulene, water-soluble copper compounds such as sodium copper chlorophyllin, chlorophyll, and copper gluconate , aluminum lactate, strontium chloride, potassium nitrate, berberine, hydroxamic acid or its derivatives, glycyrrhizic acid or its salts, glycyrrhizic acid or its derivatives,
- Dentifrice compositions having compositions shown in Tables 1 to 3 were prepared by a conventional method and evaluated by the following methods. The results are also shown in the table.
- Fluoride ion retention rate (%) ⁇ (retained fluoride ion concentration (ppm))/(fluoride ion concentration (ppm)/40) ⁇ 100 From the fluorine ion retention rate, the fluorine ion retention was evaluated according to the following evaluation criteria. Evaluation criteria ⁇ : Fluoride ion retention rate is 50% or more ⁇ : Fluoride ion retention rate is 30% or more and less than 50% ⁇ : Fluoride ion retention rate is 20% or more and less than 30% ⁇ : Fluoride ion retention rate is less than 20%
- Fluoride ion release rate (%) ⁇ (released fluorine ion concentration (ppm)) / (retained fluorine ion concentration (pp m)) ⁇ 100 From the calculated fluoride ion release rate, the fluorine release property (release amount) was evaluated.
- the fluorine ion release rates of the evaluation compositions (Examples 1 to 14) after standing for 3 minutes are all less than 20%, and the fluoride ion release rates after standing for 60 minutes are all in the range of 20 to 60%. It was confirmed that there was sustained release without immediate release. From the fluoride ion release rate after standing for 180 minutes, the fluorine releasing property was evaluated according to the following evaluation criteria. Samples rated ⁇ or ⁇ were judged to pass the fluoride release property because the fluoride ions adsorbed and retained in the mucin were gradually released by saliva.
- Fluoride ion release rate after standing for 180 minutes is 70% or more
- Fluoride ion release rate after standing for 180 minutes is 50% or more and less than 70%
- Fluoride ion release rate after standing for 180 minutes is 20% or more and less than 50%
- Fluoride ion release rate after standing for 180 minutes is less than 20%
- a prescription example is shown.
- the raw materials used are the same as above.
- Gel toothpaste (A) Potassium pyrophosphate 0.7 (B) calcium glycerophosphate 0.8 (C) sodium fluoride 0.32 (D) hydroxyethyl cellulose dimethyl diallyl ammonium chloride 0.05 Sorbit solution (70% aqueous solution) 55 Propylene glycol 3 Sodium polyacrylate 0.7 Carrageenan 0.3 Xanthan gum 0.3 Xylit 5 Coconut fatty acid amidopropyl betaine 0.3 Citric acid 0.02 Sodium citrate 0.3 Perfume composition A 0.5 Remainder of purified water Total 100.0% (A)/(C) (molar ratio): 0.28 (B)/(C) (molar ratio): 0.50 (A)/(D) mass ratio: 14 (B)/(D) mass ratio: 16 (C)/(D) mass ratio: 6.4
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Abstract
Provided is a dentifrice composition that achieves excellent intraoral fluorine ion retention, in particular at the oral mucosa, and excellent fluorine ion release, has liquid separation stability and hardening stability, and also has good storage stability. A dentifrice composition that contains (A) a water-soluble polyphosphate, (B) calcium glycerophosphate, (C) a water-soluble fluorine-containing compound, and (D) cationized cellulose.
Description
本発明は、口腔内、特に口腔粘膜へのフッ素イオンの滞留性に優れ、かつその放出性にも優れる水溶性フッ素含有化合物を含有する歯磨剤組成物に関する。
The present invention relates to a dentifrice composition containing a water-soluble fluorine-containing compound that is excellent in retention of fluoride ions in the oral cavity, particularly in the oral mucosa, and also excellent in release.
フッ化ナトリウム等のフッ素含有化合物は、再石灰化促進や脱灰抑制等の機能を有する薬用成分として、う蝕予防等の目的で歯磨剤組成物等の口腔用組成物に広く用いられている。フッ素含有化合物を効果的に作用させるには、フッ素イオンを長時間に亘って口腔内の歯面に滞留させることが有効であり、また、使用後に口腔内をうがいして水で漱ぐなどした後でも口腔内にフッ素イオンを多く残して留めておくことも重要であるが、特に歯磨剤組成物はブラッシング後の漱ぎによって洗い流されるため、口腔内に残存するフッ素イオンは微量に過ぎなかった。
Fluorine-containing compounds such as sodium fluoride are widely used in oral compositions such as dentifrice compositions for the purpose of preventing dental caries as medicinal ingredients having functions such as promoting remineralization and inhibiting demineralization. . In order for the fluorine-containing compound to act effectively, it is effective to allow the fluorine ions to remain on the tooth surface in the oral cavity for a long period of time. Although it is important to retain a large amount of fluoride ions in the oral cavity even afterward, only a very small amount of fluoride ions remained in the oral cavity because the dentifrice composition was washed away by rinsing after brushing.
歯磨剤組成物に配合したフッ素イオンの口腔内滞留性を向上させるために、再石灰化成分であるカルシウムイオン、フッ素イオンを共存させる方法があるが、カルシウムイオンとフッ素イオンは反応性が高く、共存させると歯牙に対して作用する以前に不溶性物質であるフッ化カルシウムとなり、十分な効果を発揮させることができなかった。また、特許文献1(特表平10-511956号公報)では、カルシウムイオンとフッ素イオンを口腔内で又は口腔への適用直前に当該2つの組成物を混合することにより、口腔内でフッ化カルシウムを生成させる形態の口腔用剤が提案されている。しかし、この方法では、フッ素イオンとして口腔内に入るため、すぐに唾液で流され、十分な滞留効果が発揮されず、また、2成分混合後に短時間でフッ化カルシウムが析出するため、フッ素イオンが十分に放出されず再石灰化予防効果が満足に発揮されなかった。特許文献2(特開2009-137863号公報)には、ポリリン酸塩、カルシウム塩、フッ化物塩の複合体を予め調製した組成物が提案されているが、この方法では調製面での煩雑さや歯磨製剤としての長期保存後に液状化や固化するなどの課題があった。
また、特許文献3~5(特開2015-117215号公報、特開2013-67567号公報、特開2007-320894号公報)には、歯磨剤組成物において、特定のカチオン性高分子物質を用いた、歯面にフッ素イオンを吸着・滞留させる方法が提案されているが、その滞留性やブラッシング後の残存量には未だ改善の余地があり、更なる滞留性の向上が望まれた。 In order to improve the intraoral retention of fluoride ions blended in the dentifrice composition, there is a method of coexisting calcium ions and fluoride ions, which are remineralizing components, but calcium ions and fluoride ions are highly reactive, When it coexists, it turns into an insoluble substance, calcium fluoride, before it acts on teeth, and a sufficient effect could not be exhibited. Further, in Patent Document 1 (Japanese Patent Publication No. 10-511956), by mixing calcium ions and fluoride ions in the oral cavity or immediately before application to the oral cavity, calcium fluoride is added in the oral cavity. Oral agents have been proposed in the form of producing However, in this method, since it enters the oral cavity as fluoride ions, it is immediately washed away by saliva and does not exhibit a sufficient retention effect. was not sufficiently released, and the remineralization preventive effect was not exhibited satisfactorily. Patent Document 2 (Japanese Patent Application Laid-Open No. 2009-137863) proposes a composition in which a complex of a polyphosphate, a calcium salt, and a fluoride salt is prepared in advance. There were problems such as liquefaction and solidification after long-term storage as a dentifrice preparation.
In addition, Patent Documents 3 to 5 (JP-A-2015-117215, JP-A-2013-67567, JP-A-2007-320894) disclose that a specific cationic polymeric substance is used in a dentifrice composition. However, there is still room for improvement in retention and the amount remaining after brushing, and further improvement in retention has been desired.
また、特許文献3~5(特開2015-117215号公報、特開2013-67567号公報、特開2007-320894号公報)には、歯磨剤組成物において、特定のカチオン性高分子物質を用いた、歯面にフッ素イオンを吸着・滞留させる方法が提案されているが、その滞留性やブラッシング後の残存量には未だ改善の余地があり、更なる滞留性の向上が望まれた。 In order to improve the intraoral retention of fluoride ions blended in the dentifrice composition, there is a method of coexisting calcium ions and fluoride ions, which are remineralizing components, but calcium ions and fluoride ions are highly reactive, When it coexists, it turns into an insoluble substance, calcium fluoride, before it acts on teeth, and a sufficient effect could not be exhibited. Further, in Patent Document 1 (Japanese Patent Publication No. 10-511956), by mixing calcium ions and fluoride ions in the oral cavity or immediately before application to the oral cavity, calcium fluoride is added in the oral cavity. Oral agents have been proposed in the form of producing However, in this method, since it enters the oral cavity as fluoride ions, it is immediately washed away by saliva and does not exhibit a sufficient retention effect. was not sufficiently released, and the remineralization preventive effect was not exhibited satisfactorily. Patent Document 2 (Japanese Patent Application Laid-Open No. 2009-137863) proposes a composition in which a complex of a polyphosphate, a calcium salt, and a fluoride salt is prepared in advance. There were problems such as liquefaction and solidification after long-term storage as a dentifrice preparation.
In addition, Patent Documents 3 to 5 (JP-A-2015-117215, JP-A-2013-67567, JP-A-2007-320894) disclose that a specific cationic polymeric substance is used in a dentifrice composition. However, there is still room for improvement in retention and the amount remaining after brushing, and further improvement in retention has been desired.
本発明は、上記事情に鑑みなされたもので、口腔内、特に口腔粘膜へのフッ素イオンの滞留性に優れ、その放出性にも優れる歯磨剤組成物を提供することを目的とする。
The present invention has been made in view of the above circumstances, and an object thereof is to provide a dentifrice composition which is excellent in retention of fluoride ions in the oral cavity, particularly in the oral mucosa, and which is also excellent in releasability.
本発明者らは、上記目的を達成するため鋭意検討を行った結果、水溶性フッ素含有化合物に、水溶性ポリリン酸塩とグリセロリン酸カルシウムとを併用し、更にカチオン化セルロースを組み合わせて歯磨剤組成物に配合すると、口腔内、特に口腔粘膜へのフッ素イオンの滞留性に優れ、フッ素イオンが高率で口腔内に滞留し、しかも、フッ素イオンの放出性(放出量、徐放性)に優れ、滞留したフッ素イオンが徐放し、長時間に亘って口腔内にフッ素イオンを供給でき、また、長期保存後も液分離及び固化が抑制され、良好な保存安定性となることを知見した。即ち、本発明では、(A)水溶性ポリリン酸塩、(B)グリセロリン酸カルシウム、(C)水溶性フッ素含有化合物、及び(D)カチオン化セルロースを配合した歯磨剤組成物が、口腔内、特に口腔粘膜へのフッ素イオンの滞留性に優れ、その放出性にも優れ、また、液分離安定性及び固化安定性を有し保存安定性も良いことを知見し、本発明をなすに至った。
As a result of intensive studies to achieve the above object, the present inventors have found a dentifrice composition comprising a water-soluble fluorine-containing compound, a water-soluble polyphosphate and calcium glycerophosphate, and a cationized cellulose. When blended in, the retention of fluoride ions in the oral cavity, especially in the oral mucosa, is excellent, the fluoride ions are retained in the oral cavity at a high rate, and the release of fluoride ions (release amount, sustained release) is excellent. It was found that the retained fluoride ions are gradually released, the fluoride ions can be supplied to the oral cavity over a long period of time, liquid separation and solidification are suppressed even after long-term storage, and good storage stability is achieved. That is, in the present invention, a dentifrice composition containing (A) a water-soluble polyphosphate, (B) calcium glycerophosphate, (C) a water-soluble fluorine-containing compound, and (D) a cationized cellulose is used in the oral cavity, particularly The inventors have found that the fluorine ion retains well in the oral mucosa, is excellent in its releasability, has good liquid separation stability, solidification stability, and good storage stability, and has completed the present invention.
歯磨剤組成物に配合された水溶性フッ素含有化合物のフッ素が、歯面だけでなく口腔粘膜にも十分に滞留すれば口腔内滞留性がより高まると期待されたが、口腔粘膜はムチン等の唾液タンパクで覆われているためにフッ素が吸着し難く、従来の技術では口腔粘膜にフッ素を十分に滞留させることができなかった。しかし、本発明では、(C)成分に、(A)及び(B)成分を併用し、かつ(D)成分を組み合わせることで、(D)成分によって(C)成分由来のフッ素イオンの口腔粘膜への滞留性が改善し、フッ素イオンの滞留性だけでなくその放出性も優れたものとすることができた。この場合、(D)成分によって、口腔粘膜を覆っているムチンへのフッ素イオンの吸着性が高まることでその滞留性が改善し、フッ素イオンが高率で口腔粘膜に滞留し、しかも、滞留したフッ素イオンが徐々に唾液中に放出され、唾液と接する歯面に長時間供給される。したがって、本発明の歯磨剤組成物によれば、液分離安定性及び固化安定性を確保してフッ素イオンの口腔内滞留性を向上できる。
It was expected that if the fluorine contained in the water-soluble fluorine-containing compound contained in the dentifrice composition sufficiently retained not only on the tooth surface but also on the oral mucosa, the retention in the oral cavity would be further enhanced. Since it is covered with salivary proteins, it is difficult for fluorine to be adsorbed. However, in the present invention, the components (A) and (B) are used in combination with the component (C), and the component (D) is combined. As a result, not only the retention of fluorine ions but also the releasability of fluorine ions was improved. In this case, the component (D) enhances the adsorption of fluoride ions to the mucin covering the oral mucosa, thereby improving its retention, and the fluoride ions stay in the oral mucosa at a high rate and stay. Fluoride ions are gradually released into saliva and supplied to the tooth surface in contact with saliva for a long period of time. Therefore, according to the dentifrice composition of the present invention, the liquid separation stability and the solidification stability can be ensured, and the retention of fluoride ions in the oral cavity can be improved.
後述の比較例に示すように、(A)、(B)及び(C)成分が配合され、(D)成分が配合されていないと、フッ素(フッ素イオン)滞留性及びフッ素(フッ素イオン)放出性が悪く、製剤の液分離安定性が悪く(比較例3)、(D)成分が配合されていても(A)又は(B)成分が配合されていないと、フッ素滞留性及びフッ素放出性が悪く、また、製剤の液分離安定性又は製剤の固化安定性が悪かった(比較例1、2)。これに対して、本発明の(A)、(B)、(C)及び(D)成分が配合された歯磨剤組成物(後述の実施例)は、フッ素滞留性及びフッ素放出性が優れ、製剤の液分離安定性及び固化安定性が良好であった。
As shown in comparative examples below, when components (A), (B) and (C) are blended but component (D) is not blended, fluorine (fluoride ions) retention and fluorine (fluoride ions) release are poor. The liquid separation stability of the formulation is poor (Comparative Example 3), and even if component (D) is blended, if component (A) or (B) is not blended, fluorine retention and fluorine release properties are poor. In addition, the liquid separation stability of the formulation or the solidification stability of the formulation was poor (Comparative Examples 1 and 2). On the other hand, the dentifrice compositions containing the components (A), (B), (C) and (D) of the present invention (Examples described later) are excellent in fluorine retention and fluorine release. The liquid separation stability and solidification stability of the formulation were good.
したがって、本発明は、下記の歯磨剤組成物を提供する。
〔1〕
(A)水溶性ポリリン酸塩、
(B)グリセロリン酸カルシウム、
(C)水溶性フッ素含有化合物
及び
(D)カチオン化セルロース
を含有する歯磨剤組成物。
〔2〕
(A)成分が、ピロリン酸カリウムである〔1〕記載の歯磨剤組成物。
〔3〕
(A)/(C)が、モル比として0.05~1である〔1〕又は〔2〕記載の歯磨剤組成物。
〔4〕
(B)/(C)が、モル比として0.05~1.5である〔1〕~〔3〕のいずれかに記載の歯磨剤組成物。
〔5〕
(A)成分の含有量が0.1~1.5質量%、(B)成分の含有量が0.1~2質量%、(C)成分の含有量がフッ素イオンとして500~5,000ppm、(D)成分の含有量が0.01~0.5質量%である〔1〕~〔4〕のいずれかに記載の歯磨剤組成物。
〔6〕
練歯磨剤又はジェル状歯磨剤である〔1〕~〔5〕のいずれかに記載の歯磨剤組成物。 Accordingly, the present invention provides the following dentifrice composition.
[1]
(A) a water-soluble polyphosphate;
(B) calcium glycerophosphate;
A dentifrice composition containing (C) a water-soluble fluorine-containing compound and (D) a cationized cellulose.
[2]
(A) The dentifrice composition according to [1], wherein the component is potassium pyrophosphate.
[3]
The dentifrice composition according to [1] or [2], wherein (A)/(C) has a molar ratio of 0.05 to 1.
[4]
The dentifrice composition according to any one of [1] to [3], wherein (B)/(C) is 0.05 to 1.5 as a molar ratio.
[5]
The content of component (A) is 0.1 to 1.5% by mass, the content of component (B) is 0.1 to 2% by mass, and the content of component (C) is 500 to 5,000 ppm as fluorine ions. , The dentifrice composition according to any one of [1] to [4], wherein the content of component (D) is 0.01 to 0.5% by mass.
[6]
The dentifrice composition according to any one of [1] to [5], which is a toothpaste or a gel-like dentifrice.
〔1〕
(A)水溶性ポリリン酸塩、
(B)グリセロリン酸カルシウム、
(C)水溶性フッ素含有化合物
及び
(D)カチオン化セルロース
を含有する歯磨剤組成物。
〔2〕
(A)成分が、ピロリン酸カリウムである〔1〕記載の歯磨剤組成物。
〔3〕
(A)/(C)が、モル比として0.05~1である〔1〕又は〔2〕記載の歯磨剤組成物。
〔4〕
(B)/(C)が、モル比として0.05~1.5である〔1〕~〔3〕のいずれかに記載の歯磨剤組成物。
〔5〕
(A)成分の含有量が0.1~1.5質量%、(B)成分の含有量が0.1~2質量%、(C)成分の含有量がフッ素イオンとして500~5,000ppm、(D)成分の含有量が0.01~0.5質量%である〔1〕~〔4〕のいずれかに記載の歯磨剤組成物。
〔6〕
練歯磨剤又はジェル状歯磨剤である〔1〕~〔5〕のいずれかに記載の歯磨剤組成物。 Accordingly, the present invention provides the following dentifrice composition.
[1]
(A) a water-soluble polyphosphate;
(B) calcium glycerophosphate;
A dentifrice composition containing (C) a water-soluble fluorine-containing compound and (D) a cationized cellulose.
[2]
(A) The dentifrice composition according to [1], wherein the component is potassium pyrophosphate.
[3]
The dentifrice composition according to [1] or [2], wherein (A)/(C) has a molar ratio of 0.05 to 1.
[4]
The dentifrice composition according to any one of [1] to [3], wherein (B)/(C) is 0.05 to 1.5 as a molar ratio.
[5]
The content of component (A) is 0.1 to 1.5% by mass, the content of component (B) is 0.1 to 2% by mass, and the content of component (C) is 500 to 5,000 ppm as fluorine ions. , The dentifrice composition according to any one of [1] to [4], wherein the content of component (D) is 0.01 to 0.5% by mass.
[6]
The dentifrice composition according to any one of [1] to [5], which is a toothpaste or a gel-like dentifrice.
本発明によれば、口腔内、特に口腔粘膜へのフッ素イオンの滞留性に優れ、その放出性にも優れ、また、液分離安定性及び固化安定性を有し保存安定性も良い歯磨剤組成物を提供できる。本発明の歯磨剤組成物は、口腔内をブラッシング後にうがいして水で漱いだ後でもフッ素イオンを比較的多く口腔内に残して留めておくことができ、水溶性フッ素含有化合物の再石灰化促進、脱灰抑制等の効果を十分に発揮させることもでき、う蝕予防用として好適である。
ADVANTAGE OF THE INVENTION According to the present invention, a dentifrice composition is excellent in retention of fluorine ions in the oral cavity, particularly in the oral mucosa, is also excellent in its releasability, and has good liquid separation stability, solidification stability, and storage stability. can provide things. The dentifrice composition of the present invention can retain a relatively large amount of fluoride ions in the oral cavity even after gargling and rinsing the oral cavity after brushing, and remineralization of the water-soluble fluorine-containing compound. It is also suitable for caries prevention because it can sufficiently exhibit effects such as acceleration of caries and inhibition of demineralization.
以下、本発明につき更に詳述する。
本発明の歯磨剤組成物は、(A)水溶性ポリリン酸塩、(B)グリセロリン酸カルシウム、(C)水溶性フッ素含有化合物、及び(D)カチオン化セルロースを含有する。 The present invention will be described in further detail below.
The dentifrice composition of the present invention contains (A) a water-soluble polyphosphate, (B) calcium glycerophosphate, (C) a water-soluble fluorine-containing compound, and (D) cationized cellulose.
本発明の歯磨剤組成物は、(A)水溶性ポリリン酸塩、(B)グリセロリン酸カルシウム、(C)水溶性フッ素含有化合物、及び(D)カチオン化セルロースを含有する。 The present invention will be described in further detail below.
The dentifrice composition of the present invention contains (A) a water-soluble polyphosphate, (B) calcium glycerophosphate, (C) a water-soluble fluorine-containing compound, and (D) cationized cellulose.
(A)水溶性ポリリン酸塩は、フッ素イオンの滞留性の向上作用を奏し、また、液分離抑制作用を奏する。
(A)成分として、水溶性ポリリン酸塩は、ピロリン酸、トリポリリン酸、テトラポリリン酸等の直鎖状のポリリン酸、トリメタリン酸、テトラメタリン酸、ヘキサメタリン酸等の環状のポリリン酸が挙げられ、その塩としてはナトリウム塩、カリウム塩等のアルカリ金属塩が挙げられる。中でもピロリン酸塩、トリポリリン酸塩が好ましく、より好ましくはピロリン酸塩であり、特にピロリン酸カリウムが好ましい。これらは1種単独でも2種以上を併用してもよい。 (A) The water-soluble polyphosphate has an effect of improving retention of fluorine ions and an effect of suppressing liquid separation.
As the component (A), the water-soluble polyphosphate includes linear polyphosphoric acids such as pyrophosphoric acid, tripolyphosphoric acid and tetrapolyphosphoric acid, and cyclic polyphosphoric acids such as trimetaphosphoric acid, tetrametaphosphoric acid and hexametaphosphoric acid. The salts thereof include alkali metal salts such as sodium salts and potassium salts. Among them, pyrophosphate and tripolyphosphate are preferred, pyrophosphate is more preferred, and potassium pyrophosphate is particularly preferred. These may be used singly or in combination of two or more.
(A)成分として、水溶性ポリリン酸塩は、ピロリン酸、トリポリリン酸、テトラポリリン酸等の直鎖状のポリリン酸、トリメタリン酸、テトラメタリン酸、ヘキサメタリン酸等の環状のポリリン酸が挙げられ、その塩としてはナトリウム塩、カリウム塩等のアルカリ金属塩が挙げられる。中でもピロリン酸塩、トリポリリン酸塩が好ましく、より好ましくはピロリン酸塩であり、特にピロリン酸カリウムが好ましい。これらは1種単独でも2種以上を併用してもよい。 (A) The water-soluble polyphosphate has an effect of improving retention of fluorine ions and an effect of suppressing liquid separation.
As the component (A), the water-soluble polyphosphate includes linear polyphosphoric acids such as pyrophosphoric acid, tripolyphosphoric acid and tetrapolyphosphoric acid, and cyclic polyphosphoric acids such as trimetaphosphoric acid, tetrametaphosphoric acid and hexametaphosphoric acid. The salts thereof include alkali metal salts such as sodium salts and potassium salts. Among them, pyrophosphate and tripolyphosphate are preferred, pyrophosphate is more preferred, and potassium pyrophosphate is particularly preferred. These may be used singly or in combination of two or more.
(A)成分の配合量は、組成物全体の0.1~1.5%(質量%、以下同様)が好ましく、より好ましくは0.15~1.4%、更に好ましくは0.3~1.0%である。配合量が0.1%以上であると、フッ素イオンの滞留性及びその放出性が十分に得られ、また、経時でも液分離が抑制されて十分な液分離安定性が得られる。1.5%以下であると、フッ素イオンの滞留性及びその放出性が十分に維持され、また、経時での固化が防止されて十分な固化安定性が得られる。
The amount of component (A) is preferably 0.1 to 1.5% (mass%, hereinafter the same) of the entire composition, more preferably 0.15 to 1.4%, and still more preferably 0.3 to 1.0%. When the blending amount is 0.1% or more, sufficient retention and release of fluorine ions can be obtained, and liquid separation can be suppressed over time to obtain sufficient liquid separation stability. When the content is 1.5% or less, retention and release properties of fluoride ions are sufficiently maintained, and solidification over time is prevented to obtain sufficient solidification stability.
(B)グリセロリン酸カルシウムは、フッ素イオンの滞留性の向上作用を奏し、また、固化抑制作用を奏する。
グリセロリン酸カルシウムは、天然物由来でも合成品でも使用できる。例えば、岩城製薬(株)製の商品名「グリセロリン酸カルシウム」等の市販品を使用することもできる。 (B) Calcium glycerophosphate has an effect of improving retention of fluorine ions and an effect of suppressing solidification.
Calcium glycerophosphate may be derived from natural products or synthetic products. For example, a commercially available product such as “calcium glycerophosphate” manufactured by Iwaki Seiyaku Co., Ltd. can also be used.
グリセロリン酸カルシウムは、天然物由来でも合成品でも使用できる。例えば、岩城製薬(株)製の商品名「グリセロリン酸カルシウム」等の市販品を使用することもできる。 (B) Calcium glycerophosphate has an effect of improving retention of fluorine ions and an effect of suppressing solidification.
Calcium glycerophosphate may be derived from natural products or synthetic products. For example, a commercially available product such as “calcium glycerophosphate” manufactured by Iwaki Seiyaku Co., Ltd. can also be used.
(B)グリセロリン酸カルシウムの配合量は、組成物全体の0.1~2%が好ましく、より好ましくは0.15~1.8%、特に好ましくは0.25~1.5%である。配合量が0.1%以上であると、フッ素イオンの滞留性及びその放出性が十分に得られ、また、経時での固化が防止されて十分な固化安定性が得られる。2%以下であると、フッ素イオンの滞留性及びその放出性が十分に維持され、また、経時での液分離が抑制されて十分な液分離安定性が得られる。
(B) The content of calcium glycerophosphate is preferably 0.1 to 2%, more preferably 0.15 to 1.8%, and particularly preferably 0.25 to 1.5% of the total composition. When the blending amount is 0.1% or more, sufficient retention and release of fluorine ions can be obtained, and solidification over time can be prevented to obtain sufficient solidification stability. When the content is 2% or less, the retention and release properties of fluoride ions are sufficiently maintained, and liquid separation over time is suppressed to obtain sufficient liquid separation stability.
(C)水溶性フッ素含有化合物としては、フッ化ナトリウム、モノフルオロリン酸ナトリウム、フッ化スズ等が挙げられる。
(C)水溶性フッ素含有化合物の配合量は、フッ素イオンとして、組成物全体の500~5,000ppmが好ましく、より好ましくは1,100~3,000ppmである。配合量がフッ素イオンとして500ppm以上であると、フッ素イオンの滞留性の向上効果が十分に得られ、5,000ppm以下であると、過剰摂取による斑状歯等の為害作用の発生を防止できる。
水溶性フッ素含有化合物の配合量は、供給するフッ素イオン量により異なり、例えばフッ化ナトリウムの場合、供給するフッ素イオンを500ppmにする場合、その配合量は組成物全体の0.11%となる。具体的にフッ化ナトリウムの配合量は、組成物全体の0.1%以上が好ましく、より好ましくは0.25~0.7%である。 (C) Water-soluble fluorine-containing compounds include sodium fluoride, sodium monofluorophosphate, tin fluoride and the like.
(C) The content of the water-soluble fluorine-containing compound is preferably 500 to 5,000 ppm, more preferably 1,100 to 3,000 ppm, in terms of fluorine ions, based on the total composition. When the content is 500 ppm or more in terms of fluoride ions, the retention effect of fluoride ions is sufficiently improved, and when it is 5,000 ppm or less, adverse effects such as mottled teeth due to excessive intake can be prevented.
The blending amount of the water-soluble fluorine-containing compound varies depending on the amount of fluoride ions to be supplied. For example, in the case of sodium fluoride, when the amount of fluoride ions to be supplied is 500 ppm, the amount to be blended is 0.11% of the total composition. Specifically, the content of sodium fluoride is preferably 0.1% or more, more preferably 0.25 to 0.7%, based on the total composition.
(C)水溶性フッ素含有化合物の配合量は、フッ素イオンとして、組成物全体の500~5,000ppmが好ましく、より好ましくは1,100~3,000ppmである。配合量がフッ素イオンとして500ppm以上であると、フッ素イオンの滞留性の向上効果が十分に得られ、5,000ppm以下であると、過剰摂取による斑状歯等の為害作用の発生を防止できる。
水溶性フッ素含有化合物の配合量は、供給するフッ素イオン量により異なり、例えばフッ化ナトリウムの場合、供給するフッ素イオンを500ppmにする場合、その配合量は組成物全体の0.11%となる。具体的にフッ化ナトリウムの配合量は、組成物全体の0.1%以上が好ましく、より好ましくは0.25~0.7%である。 (C) Water-soluble fluorine-containing compounds include sodium fluoride, sodium monofluorophosphate, tin fluoride and the like.
(C) The content of the water-soluble fluorine-containing compound is preferably 500 to 5,000 ppm, more preferably 1,100 to 3,000 ppm, in terms of fluorine ions, based on the total composition. When the content is 500 ppm or more in terms of fluoride ions, the retention effect of fluoride ions is sufficiently improved, and when it is 5,000 ppm or less, adverse effects such as mottled teeth due to excessive intake can be prevented.
The blending amount of the water-soluble fluorine-containing compound varies depending on the amount of fluoride ions to be supplied. For example, in the case of sodium fluoride, when the amount of fluoride ions to be supplied is 500 ppm, the amount to be blended is 0.11% of the total composition. Specifically, the content of sodium fluoride is preferably 0.1% or more, more preferably 0.25 to 0.7%, based on the total composition.
本発明では、(A)成分と(C)成分との量比を示す(A)/(C)が、モル比として好ましくは0.05~1、より好ましくは0.1~0.5、特に0.10~0.50である。また、(B)成分と(C)成分との量比を示す(B)/(C)が、モル比として好ましくは0.05~1.5、より好ましくは0.10~1である。(A)/(C)のモル比、(B)/(C)のモル比がそれぞれ上記範囲内であると、更に好ましい。これらモル比の範囲内で(C)成分を配合すると、フッ素イオンの滞留性及びその放出性がより優れ、また、液分離安定性及び固化安定性がより優れる。
In the present invention, (A)/(C), which indicates the quantitative ratio of component (A) and component (C), is preferably 0.05 to 1, more preferably 0.1 to 0.5, as a molar ratio. In particular, it is 0.10 to 0.50. Also, (B)/(C), which indicates the quantitative ratio of component (B) to component (C), is preferably 0.05 to 1.5, more preferably 0.10 to 1 as a molar ratio. More preferably, the molar ratio of (A)/(C) and the molar ratio of (B)/(C) are within the above ranges. When the component (C) is blended within these molar ratio ranges, the retention and release properties of fluorine ions are more excellent, and the liquid separation stability and solidification stability are more excellent.
(D)カチオン化セルロースは、(A)及び(B)成分と組み合わせることで、(C)成分由来のフッ素イオンの滞留性を向上し、かつその放出性を改善する作用を奏し、また、液分離安定性を改善する作用を奏する。
(D) Cationized cellulose, in combination with components (A) and (B), has the effect of improving retention of fluorine ions derived from component (C) and improving their release. It has the effect of improving the separation stability.
カチオン化セルロースは、カチオンを有するセルロース、又はカチオンを有するセルロース誘導体である。カチオン化セルロースは、対イオン(例えばハロゲンイオン(塩素イオン)、メトサルフェートイオン等)を有していてもよい。カチオン化セルロースの分子量は特に限定されない。(D)成分として、カチオン化セルロースは1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
カチオン化セルロースの例としては、ヒドロキシエチルセルロースジメチルジアリルアンモニウム塩、塩化O-[2-ヒドロキシ-3-(トリメチルアンモニオ)プロピル]ヒドロキシエチルセルロースが挙げられ、好ましくはヒドロキシエチルセルロースジメチルジアリルアンモニウム塩である。
ヒドロキシエチルセルロースジメチルジアリルアンモニウム塩は、対イオンとしては塩化物イオンが挙げられ、ヒドロキシエチルセルロースジメチルジアリルアンモニウムクロリドが好適である。
本発明で用いるカチオン化セルロースは、その2%水溶液粘度(BH型ブルックフィールド粘度計、ローターNo.2、20回転、20℃、測定時間1分)が30~3,000mPa・sであることが好ましい。
カチオン化セルロースの平均分子量は、特に限定されないが、ポリエチレングリコールを標準物質としたゲルパーミエーションクロマトグラフ(GPC)法による重量平均分子量で、好ましくは100,000~1,500,000である。窒素含有量としては0.1~3%が好ましく、より好ましくは0.5~2.5%である。
このようなカチオン化セルロースとしては、例えば、アクゾノーベル(株)から市販されているCELQUAT L-200(2%水溶液粘度:35~350mPa・s、BH型ブルックフィールド粘度計、ローターNo.2、20回転、20℃、測定時間1分)、ポリエチレングリコールを標準物質としたゲルパーミエーションクロマトグラフ(GPC)法による重量平均分子量:250,000~350,000)が挙げられ、使用できる。 Cationized cellulose is cellulose with cations or cellulose derivatives with cations. The cationized cellulose may have counterions (eg, halogen ions (chloride ions), methosulfate ions, etc.). The molecular weight of cationized cellulose is not particularly limited. As the component (D), one type of cationized cellulose may be used alone, or two or more types may be used in combination.
Examples of cationized cellulose include hydroxyethylcellulose dimethyldiallylammonium salt, O-[2-hydroxy-3-(trimethylammonio)propyl]hydroxyethylcellulose chloride, preferably hydroxyethylcellulose dimethyldiallylammonium salt.
Hydroxyethylcellulose dimethyldiallylammonium salt includes chloride ion as a counter ion, and hydroxyethylcellulose dimethyldiallylammonium chloride is preferable.
The cationized cellulose used in the present invention has a 2% aqueous solution viscosity (BH type Brookfield viscometer, rotor No. 2, 20 rotations, 20°C, measurement time 1 minute) of 30 to 3,000 mPa s. preferable.
Although the average molecular weight of the cationized cellulose is not particularly limited, it is preferably 100,000 to 1,500,000 as a weight-average molecular weight determined by gel permeation chromatography (GPC) using polyethylene glycol as a standard substance. The nitrogen content is preferably 0.1-3%, more preferably 0.5-2.5%.
Examples of such cationized cellulose include CELQUAT L-200 (2% aqueous solution viscosity: 35 to 350 mPa s, BH type Brookfield viscometer, rotor No. 2, 20 rotation, 20° C., measurement time of 1 minute), weight average molecular weight by gel permeation chromatography (GPC) method using polyethylene glycol as a standard substance: 250,000 to 350,000).
カチオン化セルロースの例としては、ヒドロキシエチルセルロースジメチルジアリルアンモニウム塩、塩化O-[2-ヒドロキシ-3-(トリメチルアンモニオ)プロピル]ヒドロキシエチルセルロースが挙げられ、好ましくはヒドロキシエチルセルロースジメチルジアリルアンモニウム塩である。
ヒドロキシエチルセルロースジメチルジアリルアンモニウム塩は、対イオンとしては塩化物イオンが挙げられ、ヒドロキシエチルセルロースジメチルジアリルアンモニウムクロリドが好適である。
本発明で用いるカチオン化セルロースは、その2%水溶液粘度(BH型ブルックフィールド粘度計、ローターNo.2、20回転、20℃、測定時間1分)が30~3,000mPa・sであることが好ましい。
カチオン化セルロースの平均分子量は、特に限定されないが、ポリエチレングリコールを標準物質としたゲルパーミエーションクロマトグラフ(GPC)法による重量平均分子量で、好ましくは100,000~1,500,000である。窒素含有量としては0.1~3%が好ましく、より好ましくは0.5~2.5%である。
このようなカチオン化セルロースとしては、例えば、アクゾノーベル(株)から市販されているCELQUAT L-200(2%水溶液粘度:35~350mPa・s、BH型ブルックフィールド粘度計、ローターNo.2、20回転、20℃、測定時間1分)、ポリエチレングリコールを標準物質としたゲルパーミエーションクロマトグラフ(GPC)法による重量平均分子量:250,000~350,000)が挙げられ、使用できる。 Cationized cellulose is cellulose with cations or cellulose derivatives with cations. The cationized cellulose may have counterions (eg, halogen ions (chloride ions), methosulfate ions, etc.). The molecular weight of cationized cellulose is not particularly limited. As the component (D), one type of cationized cellulose may be used alone, or two or more types may be used in combination.
Examples of cationized cellulose include hydroxyethylcellulose dimethyldiallylammonium salt, O-[2-hydroxy-3-(trimethylammonio)propyl]hydroxyethylcellulose chloride, preferably hydroxyethylcellulose dimethyldiallylammonium salt.
Hydroxyethylcellulose dimethyldiallylammonium salt includes chloride ion as a counter ion, and hydroxyethylcellulose dimethyldiallylammonium chloride is preferable.
The cationized cellulose used in the present invention has a 2% aqueous solution viscosity (BH type Brookfield viscometer, rotor No. 2, 20 rotations, 20°C, measurement time 1 minute) of 30 to 3,000 mPa s. preferable.
Although the average molecular weight of the cationized cellulose is not particularly limited, it is preferably 100,000 to 1,500,000 as a weight-average molecular weight determined by gel permeation chromatography (GPC) using polyethylene glycol as a standard substance. The nitrogen content is preferably 0.1-3%, more preferably 0.5-2.5%.
Examples of such cationized cellulose include CELQUAT L-200 (2% aqueous solution viscosity: 35 to 350 mPa s, BH type Brookfield viscometer, rotor No. 2, 20 rotation, 20° C., measurement time of 1 minute), weight average molecular weight by gel permeation chromatography (GPC) method using polyethylene glycol as a standard substance: 250,000 to 350,000).
(D)成分の配合量は、組成物全体の0.01~0.5%が好ましく、より好ましくは0.05~0.2%である。0.01%以上配合すると、フッ素イオンの滞留性及びその放出性が十分に得られ、また、経時でも液分離が抑制されて十分な液分離安定性が得られる。0.5%以下であると、口腔粘膜への違和感が十分に抑制される。
The blending amount of component (D) is preferably 0.01-0.5%, more preferably 0.05-0.2% of the total composition. When the content is 0.01% or more, sufficient retention and release of fluorine ions can be obtained, and liquid separation can be suppressed over time to obtain sufficient liquid separation stability. If it is 0.5% or less, discomfort to the oral mucosa is sufficiently suppressed.
また、(A)成分と(D)成分との量比を示す(A)/(D)は、質量比として1~50が好ましく、より好ましくは3~25である。
(B)成分と(D)成分との量比を示す(B)/(D)は、質量比として1~50が好ましく、より好ましくは2~30である。
(C)成分と(D)成分との量比を示す(C)/(D)は、質量比として1~20が好ましく、より好ましくは1~10である。
これら質量比の範囲内で(D)成分を配合すると、(D)成分による効果が十分に発揮され、フッ素イオンの滞留性及びその放出性がより優れ、また、液分離安定性がより優れる。 In addition, (A)/(D), which indicates the quantitative ratio of component (A) and component (D), is preferably 1-50, more preferably 3-25 as a mass ratio.
(B)/(D), which indicates the quantitative ratio of component (B) to component (D), is preferably 1-50, more preferably 2-30 as a mass ratio.
(C)/(D), which indicates the quantitative ratio between component (C) and component (D), is preferably 1-20, more preferably 1-10 as a mass ratio.
When the component (D) is blended within these mass ratio ranges, the effect of the component (D) is sufficiently exhibited, and the retention and release properties of fluorine ions are more excellent, and the liquid separation stability is more excellent.
(B)成分と(D)成分との量比を示す(B)/(D)は、質量比として1~50が好ましく、より好ましくは2~30である。
(C)成分と(D)成分との量比を示す(C)/(D)は、質量比として1~20が好ましく、より好ましくは1~10である。
これら質量比の範囲内で(D)成分を配合すると、(D)成分による効果が十分に発揮され、フッ素イオンの滞留性及びその放出性がより優れ、また、液分離安定性がより優れる。 In addition, (A)/(D), which indicates the quantitative ratio of component (A) and component (D), is preferably 1-50, more preferably 3-25 as a mass ratio.
(B)/(D), which indicates the quantitative ratio of component (B) to component (D), is preferably 1-50, more preferably 2-30 as a mass ratio.
(C)/(D), which indicates the quantitative ratio between component (C) and component (D), is preferably 1-20, more preferably 1-10 as a mass ratio.
When the component (D) is blended within these mass ratio ranges, the effect of the component (D) is sufficiently exhibited, and the retention and release properties of fluorine ions are more excellent, and the liquid separation stability is more excellent.
本発明の歯磨剤組成物は、特に練歯磨剤又はジェル状歯磨剤(研磨剤無配合)、とりわけ練歯磨剤として好適であり、また、上記成分に加えて、その他の公知成分を本発明の効果を妨げない範囲で必要に応じて配合できる。例えば、研磨剤、粘結剤、粘稠剤、界面活性剤、更に必要により着色剤、甘味料、防腐剤、香料、有効成分等を配合できる。なお、歯磨剤組成物の調製方法は、特に限定されず、剤型に応じた公知の方法でよく、例えば、(A)~(D)成分、更には任意成分、水を通常の方法で配合し、調製できる。
The dentifrice composition of the present invention is particularly suitable as a toothpaste or gel-like dentifrice (abrasive-free), especially as a toothpaste, and in addition to the above ingredients, other known ingredients of the present invention It can be blended according to need within a range that does not interfere with the effect. For example, abrasives, binders, thickeners, surfactants, and if necessary, colorants, sweeteners, preservatives, fragrances, active ingredients, etc. can be added. The method for preparing the dentifrice composition is not particularly limited, and may be a known method according to the dosage form. and can be prepared.
研磨剤は、例えば無水ケイ酸、沈降性シリカ、シリカゲル、アルミノシリケート、ジルコノシリケート等のシリカ系研磨剤、第2リン酸カルシウム・2水和物又は無水和物、第1リン酸カルシウム、第3リン酸カルシウム、第4リン酸カルシウム、ピロリン酸カルシウム等のリン酸カルシウム系化合物、炭酸カルシウム、水酸化カルシウム、水酸化アルミニウム、不溶性メタリン酸ナトリウム、第3リン酸マグネシウム、炭酸マグネシウム、硫酸カルシウム、ベントナイト、チタニウム結合ケイ酸塩、合成樹脂系研磨剤が挙げられる。中でも、シリカ系研磨剤が好ましい。
研磨剤の配合量は、組成物全体の5~60%、特に5~30%が好ましい。 Examples of abrasives include silica-based abrasives such as anhydrous silicic acid, precipitated silica, silica gel, aluminosilicate, and zirconosilicate; Calcium phosphate compounds such as tetracalcium phosphate and calcium pyrophosphate, calcium carbonate, calcium hydroxide, aluminum hydroxide, insoluble sodium metaphosphate, trimagnesium phosphate, magnesium carbonate, calcium sulfate, bentonite, titanium-bound silicate, synthetic resin Abrasives can be mentioned. Among them, silica-based abrasives are preferred.
The compounding amount of the abrasive is preferably 5 to 60%, particularly 5 to 30% of the total composition.
研磨剤の配合量は、組成物全体の5~60%、特に5~30%が好ましい。 Examples of abrasives include silica-based abrasives such as anhydrous silicic acid, precipitated silica, silica gel, aluminosilicate, and zirconosilicate; Calcium phosphate compounds such as tetracalcium phosphate and calcium pyrophosphate, calcium carbonate, calcium hydroxide, aluminum hydroxide, insoluble sodium metaphosphate, trimagnesium phosphate, magnesium carbonate, calcium sulfate, bentonite, titanium-bound silicate, synthetic resin Abrasives can be mentioned. Among them, silica-based abrasives are preferred.
The compounding amount of the abrasive is preferably 5 to 60%, particularly 5 to 30% of the total composition.
粘結剤は、有機又は無機粘結剤を配合できる。具体的には、カルボキシメチルセルロースナトリウム、メチルセルロース、ヒドロキシメチルセルロース、ヒドロキシエチルセルロース、ヒドロキシプロピルセルロース、ヒドロキシプロピルメチルセルロース、ヒドロキシメチルエチルセルロース等のセルロース誘導体、アルギン酸ナトリウム等のアルギン酸誘導体、キサンタンガム、トラガカントガム、カラヤガム、アラビアガム等のガム類、ポリアクリル酸塩、カラギーナン、ポリビニルアルコール、カルボキシビニルポリマーといった有機粘結剤、増粘性シリカ、増粘性アルミニウムシリカ、ビーガム、ラポナイト等の無機粘結剤が挙げられる。
粘結剤の配合量は、組成物全体の0.1~5%、特に0.2~3%が好ましい。なお、本発明では、特に有機粘結剤が好ましく、有機粘結剤の配合量は、組成物全体の0.1~5%、特に0.5~3%がよい。無機粘結剤、特に増粘性シリカは、フッ素イオンの滞留性の点で、配合する場合は組成物全体の5%以下、特に2%以下、とりわけ1%以下が好ましく、配合せず0%でもよい。 The binder can be an organic or inorganic binder. Specifically, cellulose derivatives such as sodium carboxymethylcellulose, methylcellulose, hydroxymethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose, hydroxymethylethylcellulose, alginic acid derivatives such as sodium alginate, xanthan gum, tragacanth gum, karaya gum, gum arabic, etc. Examples include organic binders such as gums, polyacrylates, carrageenan, polyvinyl alcohol and carboxyvinyl polymer, and inorganic binders such as thickening silica, thickening aluminum silica, veegum and laponite.
The content of the binder is preferably 0.1 to 5%, particularly 0.2 to 3%, of the total composition. In the present invention, an organic binder is particularly preferred, and the amount of the organic binder to be blended is preferably 0.1 to 5%, particularly 0.5 to 3%, of the total composition. The inorganic binder, especially the thickening silica, is preferably 5% or less, particularly 2% or less, particularly preferably 1% or less of the total composition in terms of retention of fluorine ions, and even if it is not blended, it is 0%. good.
粘結剤の配合量は、組成物全体の0.1~5%、特に0.2~3%が好ましい。なお、本発明では、特に有機粘結剤が好ましく、有機粘結剤の配合量は、組成物全体の0.1~5%、特に0.5~3%がよい。無機粘結剤、特に増粘性シリカは、フッ素イオンの滞留性の点で、配合する場合は組成物全体の5%以下、特に2%以下、とりわけ1%以下が好ましく、配合せず0%でもよい。 The binder can be an organic or inorganic binder. Specifically, cellulose derivatives such as sodium carboxymethylcellulose, methylcellulose, hydroxymethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose, hydroxymethylethylcellulose, alginic acid derivatives such as sodium alginate, xanthan gum, tragacanth gum, karaya gum, gum arabic, etc. Examples include organic binders such as gums, polyacrylates, carrageenan, polyvinyl alcohol and carboxyvinyl polymer, and inorganic binders such as thickening silica, thickening aluminum silica, veegum and laponite.
The content of the binder is preferably 0.1 to 5%, particularly 0.2 to 3%, of the total composition. In the present invention, an organic binder is particularly preferred, and the amount of the organic binder to be blended is preferably 0.1 to 5%, particularly 0.5 to 3%, of the total composition. The inorganic binder, especially the thickening silica, is preferably 5% or less, particularly 2% or less, particularly preferably 1% or less of the total composition in terms of retention of fluorine ions, and even if it is not blended, it is 0%. good.
粘稠剤は、ソルビット、キシリット、エリスリトール、マルチット、ラクチット等の糖アルコール、グリセリン、プロピレングリコール、平均分子量160~400(医薬部外品原料規格2006記載の平均分子量)のポリエチレングリコール等の多価アルコールが挙げられる。粘稠剤の配合量は、通常、組成物全体の5~60%がよい。
Viscosity agents include sugar alcohols such as sorbit, xylit, erythritol, maltit and lactit, polyhydric alcohols such as glycerin, propylene glycol, and polyethylene glycol with an average molecular weight of 160 to 400 (average molecular weight according to the Standards for Quasi-drug Ingredients 2006). is mentioned. The blending amount of the thickening agent is usually 5 to 60% of the total composition.
界面活性剤は、アニオン性界面活性剤、ノニオン性界面活性剤、両性界面活性剤を配合することができる。
アニオン性界面活性剤は、ラウリル硫酸ナトリウム、ミリスチル硫酸ナトリウム等のアルキル硫酸塩、ラウロイルサルコシンナトリウム、ミリストイルサルコシンナトリウム等のアシルサルコシン酸塩、ドデシルベンゼンスルホン酸ナトリウム、水素添加ココナッツ脂肪酸モノグリセリドモノ硫酸ナトリウム、ラウリルスルホ酢酸ナトリウムや、N-パルミトイルグルタミン酸ナトリウム等のアシルグルタミン酸塩、N-メチル-N-アシルタウリンナトリウム、N-メチル-N-アシルアラニンナトリウム、α-オレフィンスルホン酸ナトリウムが挙げられる。
ノニオン性界面活性剤は、ポリオキシエチレンアルキルエーテル(例えばアルキル基の炭素数が16~18のもの)、ポリオキシエチレン硬化ヒマシ油(例えばエチレンオキサイドの平均付加モル数が40~80のもの)、アルキルグルコシド、ポリオキシエチレンポリオキシプロピレンブロック共重合体、ポリグリセリン脂肪酸エステル、ソルビタン脂肪酸エステル、ショ糖脂肪酸エステル、アルキロールアマイド、ポリオキシエチレンソルビタンモノステアレート、ポリオキシエチレンポリオキシプロピレングリコール等が挙げられる。
両性界面活性剤は、ラウリルジメチルアミノ酢酸ベタイン、N-ヤシ油脂肪酸アシル-N-カルボキシメチル-N-ヒドロキシエチルエチレンジアミン、ヤシ油脂肪酸アミドプロピルジメチルアミノ酢酸ベタイン、ヤシ油脂肪酸アミドプロピル等が挙げられる。
界面活性剤の配合量は、通常、組成物全体の0.1~10%がよい。配合量は、歯磨剤組成物の形態、使用目的等に応じ調整でき、例えば、練歯磨剤には0.1~10%配合することができる。 Surfactants can be blended with anionic surfactants, nonionic surfactants, and amphoteric surfactants.
Anionic surfactants include alkyl sulfates such as sodium lauryl sulfate and sodium myristyl sulfate, acyl sarcosinates such as sodium lauroyl sarcosinate and sodium myristoyl sarcosinate, sodium dodecylbenzene sulfonate, hydrogenated coconut fatty acid monoglyceride monosodium sulfate, lauryl Examples include sodium sulfoacetate, acylglutamates such as sodium N-palmitoyl glutamate, sodium N-methyl-N-acyl taurine, sodium N-methyl-N-acylalanine, and sodium α-olefin sulfonate.
Nonionic surfactants include polyoxyethylene alkyl ethers (for example, alkyl groups having 16 to 18 carbon atoms), polyoxyethylene hydrogenated castor oils (for example, those having an average added mole number of ethylene oxide of 40 to 80), Alkyl glucoside, polyoxyethylene polyoxypropylene block copolymer, polyglycerol fatty acid ester, sorbitan fatty acid ester, sucrose fatty acid ester, alkylolamide, polyoxyethylene sorbitan monostearate, polyoxyethylene polyoxypropylene glycol, etc. be done.
Amphoteric surfactants include betaine lauryldimethylaminoacetate, N-coconut fatty acid acyl-N-carboxymethyl-N-hydroxyethylethylenediamine, betaine coconut amidopropyldimethylaminoacetate, and amidopropyl coconut oil.
The amount of the surfactant to be blended is usually 0.1 to 10% of the total composition. The blending amount can be adjusted depending on the form of the dentifrice composition, the purpose of use, etc. For example, 0.1 to 10% can be blended in a toothpaste.
アニオン性界面活性剤は、ラウリル硫酸ナトリウム、ミリスチル硫酸ナトリウム等のアルキル硫酸塩、ラウロイルサルコシンナトリウム、ミリストイルサルコシンナトリウム等のアシルサルコシン酸塩、ドデシルベンゼンスルホン酸ナトリウム、水素添加ココナッツ脂肪酸モノグリセリドモノ硫酸ナトリウム、ラウリルスルホ酢酸ナトリウムや、N-パルミトイルグルタミン酸ナトリウム等のアシルグルタミン酸塩、N-メチル-N-アシルタウリンナトリウム、N-メチル-N-アシルアラニンナトリウム、α-オレフィンスルホン酸ナトリウムが挙げられる。
ノニオン性界面活性剤は、ポリオキシエチレンアルキルエーテル(例えばアルキル基の炭素数が16~18のもの)、ポリオキシエチレン硬化ヒマシ油(例えばエチレンオキサイドの平均付加モル数が40~80のもの)、アルキルグルコシド、ポリオキシエチレンポリオキシプロピレンブロック共重合体、ポリグリセリン脂肪酸エステル、ソルビタン脂肪酸エステル、ショ糖脂肪酸エステル、アルキロールアマイド、ポリオキシエチレンソルビタンモノステアレート、ポリオキシエチレンポリオキシプロピレングリコール等が挙げられる。
両性界面活性剤は、ラウリルジメチルアミノ酢酸ベタイン、N-ヤシ油脂肪酸アシル-N-カルボキシメチル-N-ヒドロキシエチルエチレンジアミン、ヤシ油脂肪酸アミドプロピルジメチルアミノ酢酸ベタイン、ヤシ油脂肪酸アミドプロピル等が挙げられる。
界面活性剤の配合量は、通常、組成物全体の0.1~10%がよい。配合量は、歯磨剤組成物の形態、使用目的等に応じ調整でき、例えば、練歯磨剤には0.1~10%配合することができる。 Surfactants can be blended with anionic surfactants, nonionic surfactants, and amphoteric surfactants.
Anionic surfactants include alkyl sulfates such as sodium lauryl sulfate and sodium myristyl sulfate, acyl sarcosinates such as sodium lauroyl sarcosinate and sodium myristoyl sarcosinate, sodium dodecylbenzene sulfonate, hydrogenated coconut fatty acid monoglyceride monosodium sulfate, lauryl Examples include sodium sulfoacetate, acylglutamates such as sodium N-palmitoyl glutamate, sodium N-methyl-N-acyl taurine, sodium N-methyl-N-acylalanine, and sodium α-olefin sulfonate.
Nonionic surfactants include polyoxyethylene alkyl ethers (for example, alkyl groups having 16 to 18 carbon atoms), polyoxyethylene hydrogenated castor oils (for example, those having an average added mole number of ethylene oxide of 40 to 80), Alkyl glucoside, polyoxyethylene polyoxypropylene block copolymer, polyglycerol fatty acid ester, sorbitan fatty acid ester, sucrose fatty acid ester, alkylolamide, polyoxyethylene sorbitan monostearate, polyoxyethylene polyoxypropylene glycol, etc. be done.
Amphoteric surfactants include betaine lauryldimethylaminoacetate, N-coconut fatty acid acyl-N-carboxymethyl-N-hydroxyethylethylenediamine, betaine coconut amidopropyldimethylaminoacetate, and amidopropyl coconut oil.
The amount of the surfactant to be blended is usually 0.1 to 10% of the total composition. The blending amount can be adjusted depending on the form of the dentifrice composition, the purpose of use, etc. For example, 0.1 to 10% can be blended in a toothpaste.
着色剤は、赤色2号、赤色3号、赤色225号、赤色226号、黄色4号、黄色5号、黄色205号、青色1号、青色2号、青色201号、青色204号、緑色3号、雲母チタン、酸化チタン等が挙げられる。
甘味料は、サッカリンナトリウム、アスパルテーム、ステビオサイド、ステビアエキス、パラメトキシシンナミックアルデヒド、ネオヘスペリジンジヒドロカルコン、ペリラルチン等が挙げられる。
防腐剤は、メチルパラベン、エチルパラベン、ブチルパラベン等のパラオキシ安息香酸エステル、安息香酸ナトリウム等の安息香酸又はその塩が挙げられる。 Colorants include Red No. 2, Red No. 3, Red No. 225, Red No. 226, Yellow No. 4, Yellow No. 5, Yellow No. 205, Blue No. 1, Blue No. 2, Blue No. 201, Blue No. 204, Green 3. No. 2, mica titanium, titanium oxide, and the like.
Sweeteners include sodium saccharin, aspartame, stevioside, stevia extract, paramethoxycinnamic aldehyde, neohesperidin dihydrochalcone, perillartine and the like.
Examples of the antiseptic include paraoxybenzoic acid esters such as methylparaben, ethylparaben and butylparaben, and benzoic acid such as sodium benzoate and salts thereof.
甘味料は、サッカリンナトリウム、アスパルテーム、ステビオサイド、ステビアエキス、パラメトキシシンナミックアルデヒド、ネオヘスペリジンジヒドロカルコン、ペリラルチン等が挙げられる。
防腐剤は、メチルパラベン、エチルパラベン、ブチルパラベン等のパラオキシ安息香酸エステル、安息香酸ナトリウム等の安息香酸又はその塩が挙げられる。 Colorants include Red No. 2, Red No. 3, Red No. 225, Red No. 226, Yellow No. 4, Yellow No. 5, Yellow No. 205, Blue No. 1, Blue No. 2, Blue No. 201, Blue No. 204, Green 3. No. 2, mica titanium, titanium oxide, and the like.
Sweeteners include sodium saccharin, aspartame, stevioside, stevia extract, paramethoxycinnamic aldehyde, neohesperidin dihydrochalcone, perillartine and the like.
Examples of the antiseptic include paraoxybenzoic acid esters such as methylparaben, ethylparaben and butylparaben, and benzoic acid such as sodium benzoate and salts thereof.
香料は、ペパーミント油、スペアミント油、アニス油、ユーカリ油、ウィンターグリーン油、カシア油、クローブ油、タイム油、セージ油、レモン油、オレンジ油、ハッカ油、カルダモン油、コリアンダー油、マンダリン油、ライム油、ラベンダー油、ローズマリー油、ローレル油、カモミル油、キャラウェイ油、マジョラム油、ベイ油、レモングラス油、オリガナム油、パインニードル油、ネロリ油、ローズ油、ジャスミン油、グレープフルーツ油、スウィーティー油、柚油、イリスコンクリート、アブソリュートペパーミント、アブソリュートローズ、オレンジフラワー等の天然香料や、これら天然香料の加工処理(前溜部カット、後溜部カット、分留、液液抽出、エッセンス化、粉末香料化等)した香料、及び、メントール、カルボン、アネトール、シネオール、サリチル酸メチル、シンナミックアルデヒド、オイゲノール、3-l-メントキシプロパン-1,2-ジオール、チモール、リナロール、リナリールアセテート、リモネン、メントン、メンチルアセテート、N-置換-パラメンタン-3-カルボキサミド、ピネン、オクチルアルデヒド、シトラール、プレゴン、カルビールアセテート、アニスアルデヒド、エチルアセテート、エチルブチレート、アリルシクロヘキサンプロピオネート、メチルアンスラニレート、エチルメチルフェニルグリシデート、バニリン、ウンデカラクトン、ヘキサナール、ブタノール、イソアミルアルコール、ヘキセノール、ジメチルサルファイド、シクロテン、フルフラール、トリメチルピラジン、エチルラクテート、エチルチオアセテート等の単品香料、更に、ストロベリーフレーバー、アップルフレーバー、バナナフレーバー、パイナップルフレーバー、グレープフレーバー、マンゴーフレーバー、バターフレーバー、ミルクフレーバー、フルーツミックスフレーバー、トロピカルフルーツフレーバー等の調合香料等、歯磨剤組成物に用いられる公知の香料素材を組み合わせて使用することができる。
また、配合量も特に限定されないが、上記の香料素材は、製剤組成中に0.000001~1%使用することが好ましい。また、上記香料素材を使用した賦香用香料としては、製剤組成中に0.05~2%使用することが好ましい。 Peppermint oil, spearmint oil, anise oil, eucalyptus oil, wintergreen oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil, lime. Oil, Lavender Oil, Rosemary Oil, Laurel Oil, Chamomile Oil, Caraway Oil, Marjoram Oil, Bay Oil, Lemongrass Oil, Origanum Oil, Pine Needle Oil, Neroli Oil, Rose Oil, Jasmine Oil, Grapefruit Oil, Sweetie Oil , Yuzu Oil, Iris Concrete, Absolute Peppermint, Absolute Rose, Orange Flower, etc., and processing of these natural flavors (pre-reservoir cut, post-reservoir cut, fractional distillation, liquid-liquid extraction, essence formation, powder perfume ), and menthol, carvone, anethole, cineol, methyl salicylate, cinnamic aldehyde, eugenol, 3-l-menthoxypropane-1,2-diol, thymol, linalool, linalyl acetate, limonene, menthone , menthyl acetate, N-substituted-paramenthane-3-carboxamide, pinene, octylaldehyde, citral, pulegone, carbyl acetate, anisaldehyde, ethyl acetate, ethyl butyrate, allyl cyclohexane propionate, methyl anthranilate, ethyl methyl Phenyl glycidate, vanillin, undecalactone, hexanal, butanol, isoamyl alcohol, hexenol, dimethyl sulfide, cyclotene, furfural, trimethylpyrazine, ethyl lactate, ethyl thioacetate, etc., strawberry flavor, apple flavor, banana flavor , pineapple flavor, grape flavor, mango flavor, butter flavor, milk flavor, mixed fruit flavor, tropical fruit flavor, and other known flavor materials used in dentifrice compositions can be used in combination.
In addition, although the blending amount is not particularly limited, it is preferable to use 0.000001 to 1% of the above perfume material in the formulation composition. In addition, it is preferable to use 0.05 to 2% in the formulation composition as a perfume for perfume using the above perfume material.
また、配合量も特に限定されないが、上記の香料素材は、製剤組成中に0.000001~1%使用することが好ましい。また、上記香料素材を使用した賦香用香料としては、製剤組成中に0.05~2%使用することが好ましい。 Peppermint oil, spearmint oil, anise oil, eucalyptus oil, wintergreen oil, cassia oil, clove oil, thyme oil, sage oil, lemon oil, orange oil, peppermint oil, cardamom oil, coriander oil, mandarin oil, lime. Oil, Lavender Oil, Rosemary Oil, Laurel Oil, Chamomile Oil, Caraway Oil, Marjoram Oil, Bay Oil, Lemongrass Oil, Origanum Oil, Pine Needle Oil, Neroli Oil, Rose Oil, Jasmine Oil, Grapefruit Oil, Sweetie Oil , Yuzu Oil, Iris Concrete, Absolute Peppermint, Absolute Rose, Orange Flower, etc., and processing of these natural flavors (pre-reservoir cut, post-reservoir cut, fractional distillation, liquid-liquid extraction, essence formation, powder perfume ), and menthol, carvone, anethole, cineol, methyl salicylate, cinnamic aldehyde, eugenol, 3-l-menthoxypropane-1,2-diol, thymol, linalool, linalyl acetate, limonene, menthone , menthyl acetate, N-substituted-paramenthane-3-carboxamide, pinene, octylaldehyde, citral, pulegone, carbyl acetate, anisaldehyde, ethyl acetate, ethyl butyrate, allyl cyclohexane propionate, methyl anthranilate, ethyl methyl Phenyl glycidate, vanillin, undecalactone, hexanal, butanol, isoamyl alcohol, hexenol, dimethyl sulfide, cyclotene, furfural, trimethylpyrazine, ethyl lactate, ethyl thioacetate, etc., strawberry flavor, apple flavor, banana flavor , pineapple flavor, grape flavor, mango flavor, butter flavor, milk flavor, mixed fruit flavor, tropical fruit flavor, and other known flavor materials used in dentifrice compositions can be used in combination.
In addition, although the blending amount is not particularly limited, it is preferable to use 0.000001 to 1% of the above perfume material in the formulation composition. In addition, it is preferable to use 0.05 to 2% in the formulation composition as a perfume for perfume using the above perfume material.
有効成分としては、イソプロピルメチルフェノール、塩化セチルピリジニウム等の殺菌剤、正リン酸のカリウム塩、ナトリウム塩等の水溶性リン酸化合物、デキストラナーゼ、ムタナーゼ、アミラーゼ、プロテアーゼ等の酵素、トラネキサム酸、イプシロンアミノカプロン酸、トリクロサン、塩化リゾチーム、アルミニウムクロルヒドロキシアラントイン、ヒノキチオール、アスコルビン酸、酢酸トコフェロール、ジヒドロコレステロール、α-ビサボロール、クロルヘキシジン塩類、アズレンや、銅クロロフィリンナトリウム、クロロフィル、グルコン酸銅等の水溶性銅化合物、乳酸アルミニウム、塩化ストロンチウム、硝酸カリウム、ベルベリン、ヒドロキサム酸又はその誘導体、グリチルリチン酸又はその塩、グリチルレチン酸又はその誘導体、歯石防止剤が挙げられる。なお、上記有効成分は、本発明の効果を妨げない範囲で有効量配合することができる。
Active ingredients include bactericides such as isopropylmethylphenol and cetylpyridinium chloride, water-soluble phosphoric acid compounds such as orthophosphate potassium salts and sodium salts, enzymes such as dextranase, mutanase, amylase and protease, tranexamic acid, Epsilon aminocaproic acid, triclosan, lysozyme chloride, aluminum chlorohydroxyallantoin, hinokitiol, ascorbic acid, tocopheryl acetate, dihydrocholesterol, α-bisabolol, chlorhexidine salts, azulene, water-soluble copper compounds such as sodium copper chlorophyllin, chlorophyll, and copper gluconate , aluminum lactate, strontium chloride, potassium nitrate, berberine, hydroxamic acid or its derivatives, glycyrrhizic acid or its salts, glycyrrhizic acid or its derivatives, and anticalculus agents. In addition, the above active ingredient can be blended in an effective amount within a range that does not impair the effects of the present invention.
以下、実施例及び比較例、処方例を示し、本発明を具体的に説明するが、本発明は下記の実施例に制限されるものではない。なお、下記の例において%は特に断らない限りいずれも質量%を示す。
Examples, Comparative Examples, and Formulation Examples are shown below to specifically describe the present invention, but the present invention is not limited to the following Examples. In the following examples, % indicates % by mass unless otherwise specified.
[実施例、比較例]
表1~3に示す組成の歯磨剤組成物(練歯磨剤)を常法によって調製し、下記方法で評価した。結果を表に併記した。 [Examples, Comparative Examples]
Dentifrice compositions (toothpaste) having compositions shown in Tables 1 to 3 were prepared by a conventional method and evaluated by the following methods. The results are also shown in the table.
表1~3に示す組成の歯磨剤組成物(練歯磨剤)を常法によって調製し、下記方法で評価した。結果を表に併記した。 [Examples, Comparative Examples]
Dentifrice compositions (toothpaste) having compositions shown in Tables 1 to 3 were prepared by a conventional method and evaluated by the following methods. The results are also shown in the table.
(1)フッ素(フッ素イオン)滞留性の評価方法
フッ素(フッ素イオン)の口腔粘膜成分であるムチンへの吸着性試験により、フッ素イオンの滞留性を評価した。
10mL遠心チューブにムチン(Sigma-Aldrich社製)を0.2g添加し、更に歯磨剤組成物(精製水による40倍希釈液)を5mL加え、3分間作用させた。その後、3,000rpmで10分間遠心分離し、上清を除去した。得られたムチンに、クエン酸カリウム緩衝液を5mL加えて1分間撹拌し、ムチンに吸着・滞留したフッ素イオンを強制的に溶出させた。3,000rpmで10分間遠心分離して上清を回収し、溶液に含まれるフッ素(フッ素イオン)濃度をフッ素イオンメーター(Orion 1115000 4-Star:サーモフィッシャーサイエンティフィック(株)製)で測定し、滞留フッ素イオン濃度(ppm)を得た。
フッ素イオン滞留率を以下の式により算出した。
フッ素イオン滞留率(%)=
{(滞留フッ素イオン濃度(ppm))/(製剤に配合したフッ素イオン
濃度(ppm)/40)}×100
フッ素イオン滞留率から、下記の評価基準でフッ素イオン滞留性を評価した。
評価基準
◎:フッ素イオン滞留率が50%以上
〇:フッ素イオン滞留率が30%以上50%未満
△:フッ素イオン滞留率が20%以上30%未満
×:フッ素イオン滞留率が20%未満 (1) Evaluation Method for Fluorine (Fluoride Ion) Retention Fluoride ion retention was evaluated by an adsorption test of fluorine (fluoride ion) to mucin, which is a component of the oral mucosa.
0.2 g of mucin (manufactured by Sigma-Aldrich) was added to a 10 mL centrifuge tube, and 5 mL of a dentifrice composition (40-fold dilution with purified water) was added and allowed to act for 3 minutes. After that, it was centrifuged at 3,000 rpm for 10 minutes and the supernatant was removed. 5 mL of potassium citrate buffer was added to the obtained mucin and stirred for 1 minute to forcibly elute the fluorine ions adsorbed and retained in the mucin. After centrifugation at 3,000 rpm for 10 minutes, the supernatant was collected, and the fluorine (fluoride ion) concentration contained in the solution was measured with a fluorine ion meter (Orion 1115000 4-Star: manufactured by Thermo Fisher Scientific Co., Ltd.). , to obtain the retained fluoride ion concentration (ppm).
The fluorine ion retention rate was calculated by the following formula.
Fluoride ion retention rate (%) =
{(retained fluoride ion concentration (ppm))/(fluoride ion concentration (ppm)/40)}×100
From the fluorine ion retention rate, the fluorine ion retention was evaluated according to the following evaluation criteria.
Evaluation criteria ◎: Fluoride ion retention rate is 50% or more ○: Fluoride ion retention rate is 30% or more and less than 50% △: Fluoride ion retention rate is 20% or more and less than 30% ×: Fluoride ion retention rate is less than 20%
フッ素(フッ素イオン)の口腔粘膜成分であるムチンへの吸着性試験により、フッ素イオンの滞留性を評価した。
10mL遠心チューブにムチン(Sigma-Aldrich社製)を0.2g添加し、更に歯磨剤組成物(精製水による40倍希釈液)を5mL加え、3分間作用させた。その後、3,000rpmで10分間遠心分離し、上清を除去した。得られたムチンに、クエン酸カリウム緩衝液を5mL加えて1分間撹拌し、ムチンに吸着・滞留したフッ素イオンを強制的に溶出させた。3,000rpmで10分間遠心分離して上清を回収し、溶液に含まれるフッ素(フッ素イオン)濃度をフッ素イオンメーター(Orion 1115000 4-Star:サーモフィッシャーサイエンティフィック(株)製)で測定し、滞留フッ素イオン濃度(ppm)を得た。
フッ素イオン滞留率を以下の式により算出した。
フッ素イオン滞留率(%)=
{(滞留フッ素イオン濃度(ppm))/(製剤に配合したフッ素イオン
濃度(ppm)/40)}×100
フッ素イオン滞留率から、下記の評価基準でフッ素イオン滞留性を評価した。
評価基準
◎:フッ素イオン滞留率が50%以上
〇:フッ素イオン滞留率が30%以上50%未満
△:フッ素イオン滞留率が20%以上30%未満
×:フッ素イオン滞留率が20%未満 (1) Evaluation Method for Fluorine (Fluoride Ion) Retention Fluoride ion retention was evaluated by an adsorption test of fluorine (fluoride ion) to mucin, which is a component of the oral mucosa.
0.2 g of mucin (manufactured by Sigma-Aldrich) was added to a 10 mL centrifuge tube, and 5 mL of a dentifrice composition (40-fold dilution with purified water) was added and allowed to act for 3 minutes. After that, it was centrifuged at 3,000 rpm for 10 minutes and the supernatant was removed. 5 mL of potassium citrate buffer was added to the obtained mucin and stirred for 1 minute to forcibly elute the fluorine ions adsorbed and retained in the mucin. After centrifugation at 3,000 rpm for 10 minutes, the supernatant was collected, and the fluorine (fluoride ion) concentration contained in the solution was measured with a fluorine ion meter (Orion 1115000 4-Star: manufactured by Thermo Fisher Scientific Co., Ltd.). , to obtain the retained fluoride ion concentration (ppm).
The fluorine ion retention rate was calculated by the following formula.
Fluoride ion retention rate (%) =
{(retained fluoride ion concentration (ppm))/(fluoride ion concentration (ppm)/40)}×100
From the fluorine ion retention rate, the fluorine ion retention was evaluated according to the following evaluation criteria.
Evaluation criteria ◎: Fluoride ion retention rate is 50% or more ○: Fluoride ion retention rate is 30% or more and less than 50% △: Fluoride ion retention rate is 20% or more and less than 30% ×: Fluoride ion retention rate is less than 20%
(2)フッ素(フッ素イオン)放出性の評価方法
(1)で△以上の評価の組成(実施例1~14)に対して、ムチンから唾液へのフッ素イオンの放出量(放出率)及び徐放性について評価を行った。
10mL遠心チューブにムチン(Sigma-Aldrich社製)を0.2g添加し、更に歯磨剤組成物(精製水による40倍希釈液)を5mL加え、3分間作用させた。その後、3,000rpmで10分間遠心分離し、上清を除去した。
得られたムチンに、人工唾液(CaCl2=1.5mmol/L、KH2PO4=5.0mmol/L、酢酸=100mmol/L、NaCl=100mmol/L、残部=水;pH=7.0)を5mL加えて1分間撹拌し、3分間、60分間又は180分間静置し、ムチンに吸着・滞留したフッ素イオンを溶出させた後、各々3,000rpmで10分間遠心分離して上清を回収し、溶液に含まれるフッ素イオン濃度をフッ素イオンメーター(Orion 1115000 4-Star:サーモフィッシャーサイエンティフィック(株)製)で測定し、各々の放出フッ素イオン濃度を得た。
放出フッ素イオン濃度から、フッ素イオン放出率を以下の式により算出した。
フッ素イオン放出率(%)=
{(放出フッ素イオン濃度(ppm))/(滞留フッ素イオン濃度(pp
m))}×100
算出したフッ素イオン放出率から、フッ素放出性(放出量)について評価した。
評価の組成(実施例1~14)の3分間静置後のフッ素イオン放出率はいずれも20%未満、60分間静置後のフッ素イオン放出率はいずれも20~60%の範囲であり、即時放出せず徐放性があることを確認した。
180分間静置後のフッ素イオン放出率から、下記の評価基準でフッ素放出性を評価した。〇又は◎のものが、ムチンに吸着・滞留したフッ素イオンが唾液によって徐々に放出され、フッ素放出性が合格であると判断した。
評価基準
◎:180分間静置後のフッ素イオン放出率が70%以上
〇:180分間静置後のフッ素イオン放出率が50%以上70%未満
△:180分間静置後のフッ素イオン放出率が20%以上50%未満
×:180分間静置後のフッ素イオン放出率が20%未満 (2) Fluorine (fluoride ion) release property evaluation method For compositions evaluated as △ or higher in (1) (Examples 1 to 14), the amount (release rate) and sustained release of fluoride ions from mucin to saliva were evaluated. Release was evaluated.
0.2 g of mucin (manufactured by Sigma-Aldrich) was added to a 10 mL centrifuge tube, and 5 mL of a dentifrice composition (40-fold dilution with purified water) was added and allowed to act for 3 minutes. After that, it was centrifuged at 3,000 rpm for 10 minutes and the supernatant was removed.
Artificial saliva ( CaCl2 = 1.5 mmol/L, KH2PO4 = 5.0 mmol/L, acetic acid = 100 mmol/L, NaCl = 100 mmol/L, remainder = water; pH = 7.0) was added to the obtained mucin. ) was added and stirred for 1 minute, left to stand for 3 minutes, 60 minutes or 180 minutes to elute the fluorine ions adsorbed and retained in the mucin, and then centrifuged at 3,000 rpm for 10 minutes to remove the supernatant. After recovery, the fluoride ion concentration contained in the solution was measured with a fluoride ion meter (Orion 1115000 4-Star: manufactured by Thermo Fisher Scientific Co., Ltd.) to obtain the respective released fluoride ion concentrations.
From the released fluoride ion concentration, the fluoride ion release rate was calculated by the following formula.
Fluoride ion release rate (%) =
{(released fluorine ion concentration (ppm)) / (retained fluorine ion concentration (pp
m))}×100
From the calculated fluoride ion release rate, the fluorine release property (release amount) was evaluated.
The fluorine ion release rates of the evaluation compositions (Examples 1 to 14) after standing for 3 minutes are all less than 20%, and the fluoride ion release rates after standing for 60 minutes are all in the range of 20 to 60%. It was confirmed that there was sustained release without immediate release.
From the fluoride ion release rate after standing for 180 minutes, the fluorine releasing property was evaluated according to the following evaluation criteria. Samples rated ◯ or ⊚ were judged to pass the fluoride release property because the fluoride ions adsorbed and retained in the mucin were gradually released by saliva.
Evaluation criteria ◎: Fluoride ion release rate after standing for 180 minutes is 70% or more ○: Fluoride ion release rate after standing for 180 minutes is 50% or more and less than 70% △: Fluoride ion release rate after standing for 180 minutes is 20% or more and less than 50% ×: Fluoride ion release rate after standing for 180 minutes is less than 20%
(1)で△以上の評価の組成(実施例1~14)に対して、ムチンから唾液へのフッ素イオンの放出量(放出率)及び徐放性について評価を行った。
10mL遠心チューブにムチン(Sigma-Aldrich社製)を0.2g添加し、更に歯磨剤組成物(精製水による40倍希釈液)を5mL加え、3分間作用させた。その後、3,000rpmで10分間遠心分離し、上清を除去した。
得られたムチンに、人工唾液(CaCl2=1.5mmol/L、KH2PO4=5.0mmol/L、酢酸=100mmol/L、NaCl=100mmol/L、残部=水;pH=7.0)を5mL加えて1分間撹拌し、3分間、60分間又は180分間静置し、ムチンに吸着・滞留したフッ素イオンを溶出させた後、各々3,000rpmで10分間遠心分離して上清を回収し、溶液に含まれるフッ素イオン濃度をフッ素イオンメーター(Orion 1115000 4-Star:サーモフィッシャーサイエンティフィック(株)製)で測定し、各々の放出フッ素イオン濃度を得た。
放出フッ素イオン濃度から、フッ素イオン放出率を以下の式により算出した。
フッ素イオン放出率(%)=
{(放出フッ素イオン濃度(ppm))/(滞留フッ素イオン濃度(pp
m))}×100
算出したフッ素イオン放出率から、フッ素放出性(放出量)について評価した。
評価の組成(実施例1~14)の3分間静置後のフッ素イオン放出率はいずれも20%未満、60分間静置後のフッ素イオン放出率はいずれも20~60%の範囲であり、即時放出せず徐放性があることを確認した。
180分間静置後のフッ素イオン放出率から、下記の評価基準でフッ素放出性を評価した。〇又は◎のものが、ムチンに吸着・滞留したフッ素イオンが唾液によって徐々に放出され、フッ素放出性が合格であると判断した。
評価基準
◎:180分間静置後のフッ素イオン放出率が70%以上
〇:180分間静置後のフッ素イオン放出率が50%以上70%未満
△:180分間静置後のフッ素イオン放出率が20%以上50%未満
×:180分間静置後のフッ素イオン放出率が20%未満 (2) Fluorine (fluoride ion) release property evaluation method For compositions evaluated as △ or higher in (1) (Examples 1 to 14), the amount (release rate) and sustained release of fluoride ions from mucin to saliva were evaluated. Release was evaluated.
0.2 g of mucin (manufactured by Sigma-Aldrich) was added to a 10 mL centrifuge tube, and 5 mL of a dentifrice composition (40-fold dilution with purified water) was added and allowed to act for 3 minutes. After that, it was centrifuged at 3,000 rpm for 10 minutes and the supernatant was removed.
Artificial saliva ( CaCl2 = 1.5 mmol/L, KH2PO4 = 5.0 mmol/L, acetic acid = 100 mmol/L, NaCl = 100 mmol/L, remainder = water; pH = 7.0) was added to the obtained mucin. ) was added and stirred for 1 minute, left to stand for 3 minutes, 60 minutes or 180 minutes to elute the fluorine ions adsorbed and retained in the mucin, and then centrifuged at 3,000 rpm for 10 minutes to remove the supernatant. After recovery, the fluoride ion concentration contained in the solution was measured with a fluoride ion meter (Orion 1115000 4-Star: manufactured by Thermo Fisher Scientific Co., Ltd.) to obtain the respective released fluoride ion concentrations.
From the released fluoride ion concentration, the fluoride ion release rate was calculated by the following formula.
Fluoride ion release rate (%) =
{(released fluorine ion concentration (ppm)) / (retained fluorine ion concentration (pp
m))}×100
From the calculated fluoride ion release rate, the fluorine release property (release amount) was evaluated.
The fluorine ion release rates of the evaluation compositions (Examples 1 to 14) after standing for 3 minutes are all less than 20%, and the fluoride ion release rates after standing for 60 minutes are all in the range of 20 to 60%. It was confirmed that there was sustained release without immediate release.
From the fluoride ion release rate after standing for 180 minutes, the fluorine releasing property was evaluated according to the following evaluation criteria. Samples rated ◯ or ⊚ were judged to pass the fluoride release property because the fluoride ions adsorbed and retained in the mucin were gradually released by saliva.
Evaluation criteria ◎: Fluoride ion release rate after standing for 180 minutes is 70% or more ○: Fluoride ion release rate after standing for 180 minutes is 50% or more and less than 70% △: Fluoride ion release rate after standing for 180 minutes is 20% or more and less than 50% ×: Fluoride ion release rate after standing for 180 minutes is less than 20%
(3)保存安定性の評価方法
(3-1)製剤の液分離安定性(保存後の液分離のなさ)の評価方法
歯磨剤組成物を50gずつチューブ容器(素材:最内層が直鎖状低密度ポリエチレンからなる直径26mmのラミネートチューブ(大日本印刷(株))製)3本に充填し、40℃で1ヶ月間保存した。保存後に各チューブ容器から歯磨剤組成物を紙の上に押し出し、液分離の状態を下記の評点基準で判定した。3本の平均点を求め、下記の評価基準で製剤の液分離安定性を評価した。
評点基準
4点:液分離が全くなかった
3点:口元部に液分離がわずかに認められたが問題ないレベルだった
2点:口元部及び練表面の液分離が認められた
1点:チューブから歯磨を押し出した時、分離液が垂れだす程度に認め
られた
評価基準
◎:平均点が4.0点
〇:平均点が3.0点以上4.0点未満
△:平均点が2.0点以上3.0点未満
×:平均点が2.0点未満 (3) Method for evaluating storage stability (3-1) Method for evaluating liquid separation stability of formulation (no liquid separation after storage) 50 g of dentifrice composition in tube container (material: innermost layer is linear Three low-density polyethylene laminate tubes having a diameter of 26 mm (manufactured by Dai Nippon Printing Co., Ltd.) were filled and stored at 40° C. for 1 month. After storage, the dentifrice composition was extruded from each tube container onto paper, and the state of liquid separation was evaluated according to the following rating criteria. The average score of the three samples was obtained, and the liquid separation stability of the formulation was evaluated according to the following evaluation criteria.
Scoring criteria 4 points: no liquid separation at all 3 points: slight liquid separation was observed at the mouth, but the level was not problematic 2 points: liquid separation was observed at the mouth and kneading surface 1 point: tube When the toothpaste was pushed out from the toothpaste, the separated liquid dripped out. Evaluation criteria ◎: Average score of 4.0 points ○: Average score of 3.0 or more and less than 4.0 points △: Average score of 2.0. 0 points or more and less than 3.0 points ×: Average score is less than 2.0 points
(3-1)製剤の液分離安定性(保存後の液分離のなさ)の評価方法
歯磨剤組成物を50gずつチューブ容器(素材:最内層が直鎖状低密度ポリエチレンからなる直径26mmのラミネートチューブ(大日本印刷(株))製)3本に充填し、40℃で1ヶ月間保存した。保存後に各チューブ容器から歯磨剤組成物を紙の上に押し出し、液分離の状態を下記の評点基準で判定した。3本の平均点を求め、下記の評価基準で製剤の液分離安定性を評価した。
評点基準
4点:液分離が全くなかった
3点:口元部に液分離がわずかに認められたが問題ないレベルだった
2点:口元部及び練表面の液分離が認められた
1点:チューブから歯磨を押し出した時、分離液が垂れだす程度に認め
られた
評価基準
◎:平均点が4.0点
〇:平均点が3.0点以上4.0点未満
△:平均点が2.0点以上3.0点未満
×:平均点が2.0点未満 (3) Method for evaluating storage stability (3-1) Method for evaluating liquid separation stability of formulation (no liquid separation after storage) 50 g of dentifrice composition in tube container (material: innermost layer is linear Three low-density polyethylene laminate tubes having a diameter of 26 mm (manufactured by Dai Nippon Printing Co., Ltd.) were filled and stored at 40° C. for 1 month. After storage, the dentifrice composition was extruded from each tube container onto paper, and the state of liquid separation was evaluated according to the following rating criteria. The average score of the three samples was obtained, and the liquid separation stability of the formulation was evaluated according to the following evaluation criteria.
Scoring criteria 4 points: no liquid separation at all 3 points: slight liquid separation was observed at the mouth, but the level was not problematic 2 points: liquid separation was observed at the mouth and kneading surface 1 point: tube When the toothpaste was pushed out from the toothpaste, the separated liquid dripped out. Evaluation criteria ◎: Average score of 4.0 points ○: Average score of 3.0 or more and less than 4.0 points △: Average score of 2.0. 0 points or more and less than 3.0 points ×: Average score is less than 2.0 points
(3-2)製剤の固化安定性(保存後の固化のなさ)の評価方法
歯磨剤組成物を50gずつチューブ容器(素材:最内層が直鎖状低密度ポリエチレンからなる直径26mmのラミネートチューブ(大日本印刷(株))製)3本に充填し、40℃で1ヶ月間保存した。保存後に各チューブ容器から歯磨剤組成物を押し出し、固化の状態を下記の評点基準で判定した。3本の平均点を求め、下記の評価基準で製剤の固化安定性を評価した。
評点基準
4点:固化が全くなかった
3点:口元部に固化がわずかに認められたが問題ないレベルだった
2点:口元部及び練表面の固化が認められた
1点:チューブから歯磨を押し出せない程度に固化が認められた
評価基準
◎:平均点が4.0点
〇:平均点が3.0点以上4.0点未満
△:平均点が2.0点以上3.0点未満
×:平均点が2.0点未満 (3-2) Evaluation method for solidification stability of formulation (no solidification after storage) Tube container containing 50 g of dentifrice composition (Material: Laminated tube with a diameter of 26 mm whose innermost layer is made of linear low-density polyethylene ( (manufactured by Dai Nippon Printing Co., Ltd.) and stored at 40° C. for 1 month. After storage, the dentifrice composition was extruded from each tube container, and the state of solidification was determined according to the following rating criteria. The solidification stability of the formulation was evaluated according to the following evaluation criteria by calculating the average score of the three.
Scoring criteria 4 points: no solidification 3 points: slight solidification was observed in the mouth area, but the level was not problematic 2 points: solidification was observed in the mouth area and the kneading surface 1 point: Toothpaste was removed from the tube. Evaluation criteria where solidification was observed to the extent that it could not be extruded ◎: Average score of 4.0 points ○: Average score of 3.0 points or more and less than 4.0 points △: Average score of 2.0 points or more and 3.0 points Less than ×: average score is less than 2.0 points
歯磨剤組成物を50gずつチューブ容器(素材:最内層が直鎖状低密度ポリエチレンからなる直径26mmのラミネートチューブ(大日本印刷(株))製)3本に充填し、40℃で1ヶ月間保存した。保存後に各チューブ容器から歯磨剤組成物を押し出し、固化の状態を下記の評点基準で判定した。3本の平均点を求め、下記の評価基準で製剤の固化安定性を評価した。
評点基準
4点:固化が全くなかった
3点:口元部に固化がわずかに認められたが問題ないレベルだった
2点:口元部及び練表面の固化が認められた
1点:チューブから歯磨を押し出せない程度に固化が認められた
評価基準
◎:平均点が4.0点
〇:平均点が3.0点以上4.0点未満
△:平均点が2.0点以上3.0点未満
×:平均点が2.0点未満 (3-2) Evaluation method for solidification stability of formulation (no solidification after storage) Tube container containing 50 g of dentifrice composition (Material: Laminated tube with a diameter of 26 mm whose innermost layer is made of linear low-density polyethylene ( (manufactured by Dai Nippon Printing Co., Ltd.) and stored at 40° C. for 1 month. After storage, the dentifrice composition was extruded from each tube container, and the state of solidification was determined according to the following rating criteria. The solidification stability of the formulation was evaluated according to the following evaluation criteria by calculating the average score of the three.
Scoring criteria 4 points: no solidification 3 points: slight solidification was observed in the mouth area, but the level was not problematic 2 points: solidification was observed in the mouth area and the kneading surface 1 point: Toothpaste was removed from the tube. Evaluation criteria where solidification was observed to the extent that it could not be extruded ◎: Average score of 4.0 points ○: Average score of 3.0 points or more and less than 4.0 points △: Average score of 2.0 points or more and 3.0 points Less than ×: average score is less than 2.0 points
使用原料の詳細を下記に示す。
(A)ピロリン酸カリウム;太平化学産業(株)製
(A)トリポリリン酸ナトリウム;太平化学産業(株)製
(B)グリセロリン酸カルシウム;岩城製薬(株)製
(C)フッ化ナトリウム;ステラケミファ(株)製
(D)ヒドロキシエチルセルロースジメチルジアリルアンモニウムクロリド
;CELQUAT L-200、アクゾノーベル(株)製、
2%水溶液粘度:35~350mPa・s(BH型ブルックフィー
ルド粘度計、ローターNo.2、20回転、20℃、測定時間1分
)、ポリエチレングリコールを標準物質としたゲルパーミエーショ
ンクロマトグラフ(GPC)法による重量平均分子量:250,0
00~350,000) Details of raw materials used are shown below.
(A) potassium pyrophosphate; manufactured by Taihei Chemical Industry Co., Ltd. (A) sodium tripolyphosphate; manufactured by Taihei Chemical Industry Co., Ltd. (B) calcium glycerophosphate; manufactured by Iwaki Pharmaceutical Co., Ltd. (C) sodium fluoride; (D) hydroxyethyl cellulose dimethyl diallyl ammonium chloride; CELQUAT L-200, manufactured by Akzo Nobel Co., Ltd.,
2% aqueous solution viscosity: 35 to 350 mPa s (BH type Brookfield viscometer, rotor No. 2, 20 rotations, 20°C, measurement time 1 minute), gel permeation chromatograph using polyethylene glycol as a standard substance ( GPC) weight average molecular weight: 250,0
00 to 350,000)
(A)ピロリン酸カリウム;太平化学産業(株)製
(A)トリポリリン酸ナトリウム;太平化学産業(株)製
(B)グリセロリン酸カルシウム;岩城製薬(株)製
(C)フッ化ナトリウム;ステラケミファ(株)製
(D)ヒドロキシエチルセルロースジメチルジアリルアンモニウムクロリド
;CELQUAT L-200、アクゾノーベル(株)製、
2%水溶液粘度:35~350mPa・s(BH型ブルックフィー
ルド粘度計、ローターNo.2、20回転、20℃、測定時間1分
)、ポリエチレングリコールを標準物質としたゲルパーミエーショ
ンクロマトグラフ(GPC)法による重量平均分子量:250,0
00~350,000) Details of raw materials used are shown below.
(A) potassium pyrophosphate; manufactured by Taihei Chemical Industry Co., Ltd. (A) sodium tripolyphosphate; manufactured by Taihei Chemical Industry Co., Ltd. (B) calcium glycerophosphate; manufactured by Iwaki Pharmaceutical Co., Ltd. (C) sodium fluoride; (D) hydroxyethyl cellulose dimethyl diallyl ammonium chloride; CELQUAT L-200, manufactured by Akzo Nobel Co., Ltd.,
2% aqueous solution viscosity: 35 to 350 mPa s (BH type Brookfield viscometer, rotor No. 2, 20 rotations, 20°C, measurement time 1 minute), gel permeation chromatograph using polyethylene glycol as a standard substance ( GPC) weight average molecular weight: 250,0
00 to 350,000)
使用した香料組成物の詳細は、表4~12に示すとおりである。上記実施例において、香料組成物Aに代えて香料組成物B~Pを使用しても評価結果は同じであり、また、後述の処方例についても同様であった。
The details of the fragrance compositions used are as shown in Tables 4-12. In the above examples, the evaluation results were the same even when the perfume compositions B to P were used in place of the perfume composition A, and the formulation examples described later were also the same.
処方例を示す。使用原料は上記と同じである。
[処方例]ジェル状歯磨剤
(A)ピロリン酸カリウム 0.7
(B)グリセロリン酸カルシウム 0.8
(C)フッ化ナトリウム 0.32
(D)ヒドロキシエチルセルロースジメチルジアリルアンモニウムクロリド
0.05
ソルビット液(70%水溶液) 55
プロピレングリコール 3
ポリアクリル酸ナトリウム 0.7
カラギーナン 0.3
キサンタンガム 0.3
キシリット 5
ヤシ油脂肪酸アミドプロピルベタイン 0.3
クエン酸 0.02
クエン酸ナトリウム 0.3
香料組成物A 0.5
精製水 残部
合計 100.0%
(A)/(C)(モル比):0.28
(B)/(C)(モル比):0.50
(A)/(D) 質量比:14
(B)/(D) 質量比:16
(C)/(D) 質量比:6.4 A prescription example is shown. The raw materials used are the same as above.
[Prescription example] Gel toothpaste (A) Potassium pyrophosphate 0.7
(B) calcium glycerophosphate 0.8
(C) sodium fluoride 0.32
(D) hydroxyethyl cellulose dimethyl diallyl ammonium chloride 0.05
Sorbit solution (70% aqueous solution) 55
Propylene glycol 3
Sodium polyacrylate 0.7
Carrageenan 0.3
Xanthan gum 0.3
Xylit 5
Coconut fatty acid amidopropyl betaine 0.3
Citric acid 0.02
Sodium citrate 0.3
Perfume composition A 0.5
Remainder of purified water
Total 100.0%
(A)/(C) (molar ratio): 0.28
(B)/(C) (molar ratio): 0.50
(A)/(D) mass ratio: 14
(B)/(D) mass ratio: 16
(C)/(D) mass ratio: 6.4
[処方例]ジェル状歯磨剤
(A)ピロリン酸カリウム 0.7
(B)グリセロリン酸カルシウム 0.8
(C)フッ化ナトリウム 0.32
(D)ヒドロキシエチルセルロースジメチルジアリルアンモニウムクロリド
0.05
ソルビット液(70%水溶液) 55
プロピレングリコール 3
ポリアクリル酸ナトリウム 0.7
カラギーナン 0.3
キサンタンガム 0.3
キシリット 5
ヤシ油脂肪酸アミドプロピルベタイン 0.3
クエン酸 0.02
クエン酸ナトリウム 0.3
香料組成物A 0.5
精製水 残部
合計 100.0%
(A)/(C)(モル比):0.28
(B)/(C)(モル比):0.50
(A)/(D) 質量比:14
(B)/(D) 質量比:16
(C)/(D) 質量比:6.4 A prescription example is shown. The raw materials used are the same as above.
[Prescription example] Gel toothpaste (A) Potassium pyrophosphate 0.7
(B) calcium glycerophosphate 0.8
(C) sodium fluoride 0.32
(D) hydroxyethyl cellulose dimethyl diallyl ammonium chloride 0.05
Sorbit solution (70% aqueous solution) 55
Propylene glycol 3
Sodium polyacrylate 0.7
Carrageenan 0.3
Xanthan gum 0.3
Xylit 5
Coconut fatty acid amidopropyl betaine 0.3
Citric acid 0.02
Sodium citrate 0.3
Perfume composition A 0.5
Remainder of purified water
Total 100.0%
(A)/(C) (molar ratio): 0.28
(B)/(C) (molar ratio): 0.50
(A)/(D) mass ratio: 14
(B)/(D) mass ratio: 16
(C)/(D) mass ratio: 6.4
Claims (6)
- (A)水溶性ポリリン酸塩、
(B)グリセロリン酸カルシウム、
(C)水溶性フッ素含有化合物
及び
(D)カチオン化セルロース
を含有する歯磨剤組成物。 (A) a water-soluble polyphosphate;
(B) calcium glycerophosphate;
A dentifrice composition containing (C) a water-soluble fluorine-containing compound and (D) a cationized cellulose. - (A)成分が、ピロリン酸カリウムである請求項1記載の歯磨剤組成物。 The dentifrice composition according to claim 1, wherein the component (A) is potassium pyrophosphate.
- (A)/(C)が、モル比として0.05~1である請求項1又は2記載の歯磨剤組成物。 The dentifrice composition according to claim 1 or 2, wherein (A)/(C) is 0.05 to 1 as a molar ratio.
- (B)/(C)が、モル比として0.05~1.5である請求項1~3のいずれか1項記載の歯磨剤組成物。 The dentifrice composition according to any one of claims 1 to 3, wherein (B)/(C) is 0.05 to 1.5 as a molar ratio.
- (A)成分の含有量が0.1~1.5質量%、(B)成分の含有量が0.1~2質量%、(C)成分の含有量がフッ素イオンとして500~5,000ppm、(D)成分の含有量が0.01~0.5質量%である請求項1~4のいずれか1項記載の歯磨剤組成物。 The content of component (A) is 0.1 to 1.5% by mass, the content of component (B) is 0.1 to 2% by mass, and the content of component (C) is 500 to 5,000 ppm as fluorine ions. 5. The dentifrice composition according to any one of claims 1 to 4, wherein the content of component (D) is 0.01 to 0.5% by mass.
- 練歯磨剤又はジェル状歯磨剤である請求項1~5のいずれか1項記載の歯磨剤組成物。 The dentifrice composition according to any one of claims 1 to 5, which is a toothpaste or a gel-like dentifrice.
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CN202280040089.7A CN117529302A (en) | 2021-06-14 | 2022-06-01 | Dentifrice composition |
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JP2016098208A (en) * | 2014-11-25 | 2016-05-30 | ライオン株式会社 | Aqueous gel composition for tooth-plane application |
JP2017066036A (en) * | 2015-09-28 | 2017-04-06 | ライオン株式会社 | Liquid oral composition |
JP2020533323A (en) * | 2017-09-08 | 2020-11-19 | スリーエム イノベイティブ プロパティズ カンパニー | Aqueous Oral Care Fluoride Treatment Compositions and Methods |
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