WO1998006377A1 - Oral compositions - Google Patents
Oral compositions Download PDFInfo
- Publication number
- WO1998006377A1 WO1998006377A1 PCT/US1997/013042 US9713042W WO9806377A1 WO 1998006377 A1 WO1998006377 A1 WO 1998006377A1 US 9713042 W US9713042 W US 9713042W WO 9806377 A1 WO9806377 A1 WO 9806377A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- water
- herbal
- chlorophenol
- extraction
- phenol
- Prior art date
Links
- 239000000203 mixture Substances 0.000 title claims description 37
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000000605 extraction Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 239000000284 extract Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 11
- 241000205585 Aquilegia canadensis Species 0.000 claims description 10
- 241000099774 Cuscuta salina Species 0.000 claims description 10
- 239000006049 herbal material Substances 0.000 claims description 9
- 239000012676 herbal extract Substances 0.000 claims description 8
- 239000003242 anti bacterial agent Substances 0.000 claims description 2
- 238000003809 water extraction Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 claims 1
- 238000002137 ultrasound extraction Methods 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 27
- 239000000377 silicon dioxide Substances 0.000 description 13
- 239000000463 material Substances 0.000 description 12
- 239000003795 chemical substances by application Substances 0.000 description 11
- 239000000606 toothpaste Substances 0.000 description 9
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 8
- 239000000551 dentifrice Substances 0.000 description 8
- 208000028169 periodontal disease Diseases 0.000 description 8
- 239000000796 flavoring agent Substances 0.000 description 7
- 235000008216 herbs Nutrition 0.000 description 7
- 239000002324 mouth wash Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000003082 abrasive agent Substances 0.000 description 6
- 239000003906 humectant Substances 0.000 description 6
- 210000000214 mouth Anatomy 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 6
- 235000003599 food sweetener Nutrition 0.000 description 5
- 208000007565 gingivitis Diseases 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000003765 sweetening agent Substances 0.000 description 5
- 229940034610 toothpaste Drugs 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 230000002882 anti-plaque Effects 0.000 description 4
- 235000013355 food flavoring agent Nutrition 0.000 description 4
- 244000005700 microbiome Species 0.000 description 4
- -1 noniontc Chemical group 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 239000013543 active substance Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 210000004268 dentin Anatomy 0.000 description 3
- 239000003995 emulsifying agent Substances 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- WKEDVNSFRWHDNR-UHFFFAOYSA-N salicylanilide Chemical compound OC1=CC=CC=C1C(=O)NC1=CC=CC=C1 WKEDVNSFRWHDNR-UHFFFAOYSA-N 0.000 description 3
- 229950000975 salicylanilide Drugs 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 229940083542 sodium Drugs 0.000 description 3
- 239000000600 sorbitol Substances 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- NKTOLZVEWDHZMU-UHFFFAOYSA-N 2,5-xylenol Chemical compound CC1=CC=C(C)C(O)=C1 NKTOLZVEWDHZMU-UHFFFAOYSA-N 0.000 description 2
- NXXYKOUNUYWIHA-UHFFFAOYSA-N 2,6-Dimethylphenol Chemical compound CC1=CC=CC(C)=C1O NXXYKOUNUYWIHA-UHFFFAOYSA-N 0.000 description 2
- YCOXTKKNXUZSKD-UHFFFAOYSA-N 3,4-xylenol Chemical compound CC1=CC=C(O)C=C1C YCOXTKKNXUZSKD-UHFFFAOYSA-N 0.000 description 2
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 2
- 241000208838 Asteraceae Species 0.000 description 2
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-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
- 241000220485 Fabaceae Species 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 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 2
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- 244000269722 Thea sinensis Species 0.000 description 2
- 235000006468 Thea sinensis Nutrition 0.000 description 2
- 208000008312 Tooth Loss Diseases 0.000 description 2
- 206010044029 Tooth deposit Diseases 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 235000020279 black tea Nutrition 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 description 2
- 229940074393 chlorogenic acid Drugs 0.000 description 2
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 description 2
- 235000001368 chlorogenic acid Nutrition 0.000 description 2
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000003412 degenerative effect Effects 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 210000004195 gingiva Anatomy 0.000 description 2
- 235000009569 green tea Nutrition 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000007937 lozenge Substances 0.000 description 2
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229940051866 mouthwash Drugs 0.000 description 2
- QWVGKYWNOKOFNN-UHFFFAOYSA-N o-cresol Chemical compound CC1=CC=CC=C1O QWVGKYWNOKOFNN-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000020333 oolong tea Nutrition 0.000 description 2
- 239000013588 oral product Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 2
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 2
- 235000019204 saccharin Nutrition 0.000 description 2
- 229940081974 saccharin Drugs 0.000 description 2
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 description 2
- 210000004872 soft tissue Anatomy 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 210000001519 tissue Anatomy 0.000 description 2
- 239000000230 xanthan gum Substances 0.000 description 2
- 229920001285 xanthan gum Polymers 0.000 description 2
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- 229940082509 xanthan gum Drugs 0.000 description 2
- 150000003751 zinc Chemical class 0.000 description 2
- KUFFULVDNCHOFZ-UHFFFAOYSA-N 2,4-xylenol Chemical compound CC1=CC=C(O)C(C)=C1 KUFFULVDNCHOFZ-UHFFFAOYSA-N 0.000 description 1
- FEDAWOPGNZDRQW-UHFFFAOYSA-N 2-benzyl-4-chlorobenzene-1,3-diol 2-(3-phenylpropyl)benzene-1,3-diol Chemical compound ClC1=C(C(=C(O)C=C1)CC1=CC=CC=C1)O.C1(=CC=CC=C1)CCCC1=C(O)C=CC=C1O FEDAWOPGNZDRQW-UHFFFAOYSA-N 0.000 description 1
- RKDMDAVSHRCXQZ-UHFFFAOYSA-N 2-benzylbenzene-1,3-diol Chemical compound OC1=CC=CC(O)=C1CC1=CC=CC=C1 RKDMDAVSHRCXQZ-UHFFFAOYSA-N 0.000 description 1
- TYBHZVUFOINFDV-UHFFFAOYSA-N 2-bromo-6-[(3-bromo-5-chloro-2-hydroxyphenyl)methyl]-4-chlorophenol Chemical compound OC1=C(Br)C=C(Cl)C=C1CC1=CC(Cl)=CC(Br)=C1O TYBHZVUFOINFDV-UHFFFAOYSA-N 0.000 description 1
- BRYHBLAGEXUHSL-UHFFFAOYSA-N 2-butan-2-yl-4-chloro-5-methylphenol Chemical compound CCC(C)C1=CC(Cl)=C(C)C=C1O BRYHBLAGEXUHSL-UHFFFAOYSA-N 0.000 description 1
- LCQXXVFFJHBYME-UHFFFAOYSA-N 2-butyl-4-hydroxybenzoic acid Chemical compound CCCCC1=CC(O)=CC=C1C(O)=O LCQXXVFFJHBYME-UHFFFAOYSA-N 0.000 description 1
- IDORTRMORJMPID-UHFFFAOYSA-N 2-butylbenzene-1,3-diol 2-ethylbenzene-1,3-diol 2-propylbenzene-1,3-diol Chemical compound C(CCC)C1=C(O)C=CC=C1O.C(CC)C1=C(O)C=CC=C1O.C(C)C1=C(O)C=CC=C1O IDORTRMORJMPID-UHFFFAOYSA-N 0.000 description 1
- HKHXLHGVIHQKMK-UHFFFAOYSA-N 2-chloro-m-cresol Chemical compound CC1=CC=CC(O)=C1Cl HKHXLHGVIHQKMK-UHFFFAOYSA-N 0.000 description 1
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- PQSXNIMHIHYFEE-UHFFFAOYSA-N 4-(1-phenylethyl)benzene-1,3-diol Chemical compound C=1C=C(O)C=C(O)C=1C(C)C1=CC=CC=C1 PQSXNIMHIHYFEE-UHFFFAOYSA-N 0.000 description 1
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- 241000205578 Thalictrum Species 0.000 description 1
- 241001122767 Theaceae Species 0.000 description 1
- 229920001615 Tragacanth Polymers 0.000 description 1
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- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 description 1
- 241000234299 Zingiberaceae Species 0.000 description 1
- YGCFIWIQZPHFLU-UHFFFAOYSA-N acesulfame Chemical compound CC1=CC(=O)NS(=O)(=O)O1 YGCFIWIQZPHFLU-UHFFFAOYSA-N 0.000 description 1
- 229960005164 acesulfame Drugs 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- CKGWFZQGEQJZIL-UHFFFAOYSA-N amylmetacresol Chemical compound CCCCCC1=CC=C(C)C=C1O CKGWFZQGEQJZIL-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000002272 anti-calculus Effects 0.000 description 1
- 230000000675 anti-caries Effects 0.000 description 1
- 230000003610 anti-gingivitis Effects 0.000 description 1
- 239000000605 aspartame Substances 0.000 description 1
- IAOZJIPTCAWIRG-QWRGUYRKSA-N aspartame Chemical compound OC(=O)C[C@H](N)C(=O)N[C@H](C(=O)OC)CC1=CC=CC=C1 IAOZJIPTCAWIRG-QWRGUYRKSA-N 0.000 description 1
- 235000010357 aspartame Nutrition 0.000 description 1
- 229960003438 aspartame Drugs 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid group Chemical group C(C1=CC=CC=C1)(=O)O WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 239000003124 biologic agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- FQUNFJULCYSSOP-UHFFFAOYSA-N bisoctrizole Chemical compound N1=C2C=CC=CC2=NN1C1=CC(C(C)(C)CC(C)(C)C)=CC(CC=2C(=C(C=C(C=2)C(C)(C)CC(C)(C)C)N2N=C3C=CC=CC3=N2)O)=C1O FQUNFJULCYSSOP-UHFFFAOYSA-N 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- JUNWLZAGQLJVLR-UHFFFAOYSA-J calcium diphosphate Chemical compound [Ca+2].[Ca+2].[O-]P([O-])(=O)OP([O-])([O-])=O JUNWLZAGQLJVLR-UHFFFAOYSA-J 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 229940043256 calcium pyrophosphate Drugs 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 229920003090 carboxymethyl hydroxyethyl cellulose Polymers 0.000 description 1
- 235000010418 carrageenan Nutrition 0.000 description 1
- 239000000679 carrageenan Substances 0.000 description 1
- 229920001525 carrageenan Polymers 0.000 description 1
- 229940113118 carrageenan Drugs 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 229940112822 chewing gum Drugs 0.000 description 1
- 235000015218 chewing gum Nutrition 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000010634 clove oil Substances 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 239000000625 cyclamic acid and its Na and Ca salt Substances 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000008121 dextrose Substances 0.000 description 1
- 235000019821 dicalcium diphosphate Nutrition 0.000 description 1
- RBLGLDWTCZMLRW-UHFFFAOYSA-K dicalcium;phosphate;dihydrate Chemical compound O.O.[Ca+2].[Ca+2].[O-]P([O-])([O-])=O RBLGLDWTCZMLRW-UHFFFAOYSA-K 0.000 description 1
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical class C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical class [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 235000019820 disodium diphosphate Nutrition 0.000 description 1
- GYQBBRRVRKFJRG-UHFFFAOYSA-L disodium pyrophosphate Chemical compound [Na+].[Na+].OP([O-])(=O)OP(O)([O-])=O GYQBBRRVRKFJRG-UHFFFAOYSA-L 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 210000002919 epithelial cell Anatomy 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- VYKKDKFTDMVOBU-UHFFFAOYSA-N flusalan Chemical compound OC1=C(Br)C=C(Br)C=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 VYKKDKFTDMVOBU-UHFFFAOYSA-N 0.000 description 1
- 229950004696 flusalan Drugs 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 229960002737 fructose Drugs 0.000 description 1
- 208000024693 gingival disease Diseases 0.000 description 1
- 229960001031 glucose Drugs 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000009036 growth inhibition Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000001050 hortel pimenta Nutrition 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 229940071826 hydroxyethyl cellulose Drugs 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 208000027866 inflammatory disease Diseases 0.000 description 1
- 230000002757 inflammatory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 235000010494 karaya gum Nutrition 0.000 description 1
- 235000021374 legumes Nutrition 0.000 description 1
- 210000000265 leukocyte Anatomy 0.000 description 1
- 210000003041 ligament Anatomy 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Chemical class 0.000 description 1
- 239000002184 metal Chemical class 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- ASHGTJPOSUFTGB-UHFFFAOYSA-N methyl resorcinol Natural products COC1=CC=CC(O)=C1 ASHGTJPOSUFTGB-UHFFFAOYSA-N 0.000 description 1
- OSWPMRLSEDHDFF-UHFFFAOYSA-N methyl salicylate Chemical compound COC(=O)C1=CC=CC=C1O OSWPMRLSEDHDFF-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920001206 natural gum Polymers 0.000 description 1
- 239000003605 opacifier Substances 0.000 description 1
- NRZWYNLTFLDQQX-UHFFFAOYSA-N p-tert-Amylphenol Chemical compound CCC(C)(C)C1=CC=C(O)C=C1 NRZWYNLTFLDQQX-UHFFFAOYSA-N 0.000 description 1
- HXDOZKJGKXYMEW-UHFFFAOYSA-N para-ethyl phenol Natural products CCC1=CC=C(O)C=C1 HXDOZKJGKXYMEW-UHFFFAOYSA-N 0.000 description 1
- IWDCLRJOBJJRNH-UHFFFAOYSA-N para-hydroxytoluene Natural products CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 description 1
- 239000006072 paste Substances 0.000 description 1
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
- 210000002379 periodontal ligament Anatomy 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 229940106025 phenylethyl resorcinol Drugs 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229940045916 polymetaphosphate Drugs 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000011321 prophylaxis Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 210000001581 salivary duct Anatomy 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- 229960001462 sodium cyclamate Drugs 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 229940045919 sodium polymetaphosphate Drugs 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000271 synthetic detergent Substances 0.000 description 1
- 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 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 229960003500 triclosan Drugs 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000009637 wintergreen oil Substances 0.000 description 1
- 239000000811 xylitol Substances 0.000 description 1
- 235000010447 xylitol Nutrition 0.000 description 1
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 229960002675 xylitol Drugs 0.000 description 1
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 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
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic 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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
-
- 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
Definitions
- the present invention relates to method of manufacturing oral compositions containing combinations of herbal materials (preferably extracts thereof) or herbal matenals mixed with water insoluble noncationic agents, as antiplaque, anticalculus and antica ⁇ es agents
- Plaque induced diseases including pe ⁇ odontitis and gingivitis, are believed to involve anaerobic bactenai infections
- Periodontal disease affects the pe ⁇ odontium, which is the investing and supporting tissue surrounding a tooth (i e , the penodontal ligament, the gingiva, and the alveolar bone)
- Gingivitis and penodontitis are inflammatory disorders of the gingiva and the periodontal ligament, respectively
- Gingivosis and pe ⁇ odontosis are more severe conditions involving degenerative disorders of the tissue
- Combinations of inflammatory and degenerative conditions are termed penodontitis complex
- Periodontal disease is a major cause of tooth loss in adults Tooth loss from periodontal disease is a significant problem beginning at age 35, but even by age 15 it is estimated that about 4 out of 5 persons already have gingivitis and 4 out of 10 have penodontitis
- Dental calculus or tartar as it is sometimes called, is a deposit which forms on the surfaces of the teeth at the gingival margin Supragingival calculus appears principally in the areas near the orifices of the salivary ducts; e g , on the lingual surfaces of the lower anterior teeth and on the buccal surfaces of the upper first and second molars, and on the distal surfaces of the posterior molars
- Mature calculus consists of an inorganic portion which is largely calcium phosphate arranged in a hydroxyapatite crystal lattice structure similar to bone, enamel and dentine
- An organic portion is also present and consists of desquamated epithelial cells, leukocytes, salivary sediment, food debris and various types of microorganisms
- the chemical approach to calculus inhibition generally involves chelation of calcium ions and/or crystal growth inhibition which prevents the calculus from forming and/or breaks down mature calculus by removing calcium
- T ⁇ closan and herbal materials have been disclosed individually for use in oral products to combat plaque and gingivitis
- compositions of the present invention comprise water insoluble noncationic and/or specific herbal extract materials obtained using the disclosed process
- safety and effective amount means sufficient amount of material to provide the desired benefit while being safe to the hard and soft tissues of the oral cavity
- compositions of this invention are meant that various additional components can be conjointly employed in the compositions of this invention as long as the listed materials perform their intended functions
- acceptable earner is meant a suitable earner which can be used to apply the present agent(s) to the oral cavity without undue toxicity, irritation, allergic response and the like, commensurate with a reasonable benefit/risk ratio
- Water Insoluble Noncationic Agents Given below are examples of antibacterial agents useful in the compositions of the present invention which are water insoluble and noncationic.
- Phenolic Compounds including phenol and its homologs, mono- and poly-alkyl and aromatic halophenols, resorcinol and its derivatives, bisphenolic compounds and halogenated salicylanilides).
- Halogenated Salicylanilides 4',5-d ⁇ bromosal ⁇ cyian ⁇ l ⁇ de 3,4',5-tr ⁇ chlorosalcylan ⁇ i ⁇ de 3,4',5-tr ⁇ bromosal ⁇ cylan ⁇ l ⁇ de 2,3,3',5-tetrachlorosal ⁇ cylan ⁇ l ⁇ de 3, 3', 5-t ⁇ chlorosal ⁇ cy lani de 3,5-d ⁇ bromo-3'-tr ⁇ fiuoromethyl salicylanilide 5-n-octanoyl-3'-t ⁇ fluoromethyl sal ⁇ cylan ⁇ l ⁇ de 3, 5-d ⁇ bromo-4'-tr ⁇ fluoromethyl salicylanilide 3,5-d ⁇ bromo-3'-tnfluoromethyl salicylanilide
- the water insoluble noncationic agent when present, is present in the oral compositions of the present invention in an effective antiplaque amount, typically about 0 005-5% by weight, preferably about 0 005-1%
- the agent is substantially water-insoluble, meaning that its solubility is less than about 1% by weight in water at 25°C and may be even less than about 0 1% If an lonizable group is present solubility is determined at a pH at which lonization does not occur
- the extracts of herbal materials useful in the development described and claimed herein are extracts of honeysuckle flowers, extracts of golden thread, or mixtures thereof
- One of the active agents in golden thread is berbenne
- a reference disclosing berbenne is U S 5,407,921 April 18, 1995, to Katsuragi et al incorporated herein by reference in its entirety
- Another patent disclosing berbenne is U S Patent 4,735,945, April 5, 1988, to Sakamoto et al also incorporated by reference herein in its entirety
- Golden thread and honeysuckle flowers are natural materials and can be obtained from the plants themselves or the active components can be synthesized if desired
- a supplier of these herbal materials is East Earth Herb, Inc , Eugene, Oregon
- An active component of golden thread, berbenne, and of honeysuckle flowers, chlorogenic acid can be obtained from a number of different sources These for berbenne include the following
- Honeysuckle flower substitutes include the following which are all mate ⁇ als which contain chlorogenic acid and/or luteo n flavonoids
- the carrier for the active component(s) can be any vehicle suitable for use in the oral cavity
- Such carriers include the usual components of mouthwashes, toothpastes, tooth powders, prophylaxis pastes, lozenges, gums and the like and are more fully described hereinafter. Dentifrices and mouthwashes are the preferred systems.
- compositions may contain other antiplaque/gingivitis agents such as quaternary ammonium compounds, water, sta ⁇ nous salts and zinc salts These types of agents are described in U.S Patent 4,656,031 , April 7, 1987 to Lane et al , and U S. Patent 5,004,597, April 2, 1991 to Majeti et al All incorporated herein by reference in their entirety
- the abrasive polishing material contemplated for use in the present toothpaste part invention can be any material which does not excessively abrade dentin
- silicas including gels and precipitates, calcium carbonate, dicalcium orthophosphate dihydrate, calcium pyrophosphate, t ⁇ calcium phosphate, calcium polymetaphosphate, insoluble
- Silica dental abrasives of various types, can provide the unique benefits of exceptional dental cleaning and polishing performance without unduly abrading tooth enamel or dentin Silica abrasive materials are also exceptionally compatible with sources of soluble fluoride and polyphosphonates For these reasons they are preferred for use herein
- the silica abrasive can be precipitated silica or silica gels such as the silica xerogels described in Pader et al , U S Patent No 3,538,230, issued March 2, 1970 and DiGiu o, U S Patent No 3,862,307, June 21 , 1975, both incorporated herein by reference Preferred are the silica xerogels marketed under the tradename "Syloid" by the W R Grace & Company, Davison Chemical Division Preferred precipitated silica materials include those marketed by the J M Huber Corporation under the tradename, "Zeodent", particularly the silica carrying the designation "Zeodent 119" These silica abrasives are described in U S Patent No 4,340,583, July 29, 1982, incorporated here
- the abrasive in the compositions described herein is present at a level of from about 6% to about 70%, preferably from about 15% to about 25% when the dentifrice is a toothpaste Higher levels, as high as 90%, may be used if the composition is a toothpowder
- Flavoring agents can also be added to dentifrice compositions Suitable flavoring agents include oil of wintergreen, oil of peppermint, oil of spearmint, and oil of clove Sweetening agents which can be used include aspartame, acesulfame, saccharin, dextrose, levulose and sodium cyclamate Flavoring and sweetening agents are generally used in dentifrices at levels of from about 0 005% to about 2% by weight
- Dentifrice compositions can also contain emulsifying agents Suitable emulsifying agents are those which are reasonably stable and foam throughout a wide pH range, including nonsoap anionic, noniontc, cationic, zwitte ⁇ onic and amphote ⁇ c organic synthetic detergents Many of these suitable surfactants are disclosed by Gieske et al in U S Patent No 4,051 ,234, September 27, 1977, incorporated herein by reference
- Water is also present in the toothpastes of this invention
- Water employed in the preparation of commercially suitable toothpastes should preferably be deionized and free of organic impurities
- Water generally comprises from about 10% to 50%, preferably from about 20% to 40%, by weight of the toothpaste compositions herein These amounts of water include
- thickening agents are carboxyvinyl polymers of the type mentioned previously herein, xanthan gum, carrageenan, hydroxyethyl cellulose and water soluble salts of cellulose ethers such as sodium carboxymethyl cellulose and sodium carboxymethyl hydroxyethyl cellulose
- Natural gums such as gum karaya, gum arable, and gum tragacanth can also be used
- Colloidal magnesium aluminum silicate or finely divided silica can be used as part of the thickening agent to further improve texture
- Thickening agents in an amount from 0 10% to 5 0% by weight of the total composition can be used
- humectant matenal in a toothpaste to keep it from hardening
- Suitable humectants include glycerin, xylitol sorbitol, and other edible polyhydnc alcohols at a level of from about 5% to about 70%
- Mouthwashes generally comprise from about 20 1 to about 2 1 of a water/ethyl alcohol solution and preferably other ingredients such as flavor, sweeteners, humectants and sudsing agents such as those mentioned above for dentifrices
- the humectants give a moist feel to the mouth
- the mouthwashes of the invention comprise 0% to 60% (preferably 10% to 25%) ethyl alcohol, 0% to 20% (preferably 5% to 20%) of a humectant, 0% to 2% (preferably 0 01% to 0 15%) emulsifying agent, 0% to 0 5% (preferably 0 005% to 0 06%) sweetening agent such as saccharin, 0% to 0 3% (preferably 0 03% to 0 3%) flavoring agent, and the balance water
- pyrophosphate salts such as those described in U S 4,515,772, May 7, 1985 to Parran et al incorporated herein by reference
- alkali metal bicarbonate such as sodium bicarbonate
- a peroxide compound in separate compartments such as disclosed in U S 4,849,213 and U S 4,528,180, both to Schaeffer, incorporated herein by reference in their entirety
- the pH of the present compositions and/or its pH in the mouth can be any pH which is safe for the mouth's hard and soft tissues Such pH's are generally from about 3 to about 10 preferably from about 4 to about 8 5 METHOD OF MANUFACTURE
- compositions of the present invention can be made using methods which are common in the oral products area
- toothpaste compositions may be prepared by mixing part of the humectant and water together and heating to 66 0 -71°C
- the fluoride source, if present, is then added along with the sweetener, the herbal materials are then added followed by the opacifier and the flavor
- the herbal extracts useful in the present inventions are formed using the processes set forth below
- a Fitzmill comminuting mill is alternately used to a Retschmill for specific milling or reduced sizing needs (e g , coarse g ⁇ nding or cryogenic milling) Any grinding operation that achieves the respective particle size for extraction is acceptable
- Crude herb extractibi ty is a critical function of exposed surface area of crude herb powder to water mass ratio
- a singular particle size is preferred for process control
- milling produces a mix of coarse and fine dust particulates
- Suitable alternate extraction process for developing this water soluble extract include use of ultrasonic water extraction systems which can provide equivalent quality, depending on the herb, with up to 94% faster process cycles
- Other suitable extraction processes include hydrolysis extracting reactors, fixed bed extracting reactors, desorption extraction columns,
- Water-extracted herbal liquid is filtered (e g , 5-100 ⁇ filter cartridge, fine screen or cheesecloth) or centnfuged to remove coarse and/or insoluble particulates
- Suitable driers that are used include fluidized bed, freeze d ⁇ er, vacuum plate, spray, drum- type and flash driers Drying efficiency is controlled for water content ( ⁇ 10%) and free water considerations ( ⁇ 0 80) to achieve shelf-stability Yield of soluble powder from the drying process is used as key to optimize herb water mass formula for extraction
- Dried pure solid herbal extract powders are sized and packaged for shipment
- a dessicating-mate ⁇ als such as a silica gel or other suitable FDA-approved, drying agent can be used to control relative humidity and to improve shelf-life
- Tnclosan 99% (irgacare MP) 0280 Carbopol 956 0250
- the herbs may be varied using levels set forth herein before Additionally, the compositions may contain other antiplaque/antigingivitis or anticaries components, such as black tea, oolong tea, green tea, quaternary ammonium compounds, and metal salts such as stannous salts and zinc salts Furthermore, members of the Ericaceae family may be used Green, oolong, and black teas are members of the general tea family (Camillia Sinenis) and may also be used in the compositions of the present invention
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Abstract
The present invention relates to a preferred method of herbal extraction, and drying.
Description
ORAL COMPOSITIONS
TECHNICAL FIELD
The present invention relates to method of manufacturing oral compositions containing combinations of herbal materials (preferably extracts thereof) or herbal matenals mixed with water insoluble noncationic agents, as antiplaque, anticalculus and anticaπes agents
Plaque induced diseases, including peπodontitis and gingivitis, are believed to involve anaerobic bactenai infections Periodontal disease affects the peπodontium, which is the investing and supporting tissue surrounding a tooth (i e , the penodontal ligament, the gingiva, and the alveolar bone) Gingivitis and penodontitis are inflammatory disorders of the gingiva and the periodontal ligament, respectively Gingivosis and peπodontosis are more severe conditions involving degenerative disorders of the tissue Combinations of inflammatory and degenerative conditions are termed penodontitis complex
Periodontal disease is a major cause of tooth loss in adults Tooth loss from periodontal disease is a significant problem beginning at age 35, but even by age 15 it is estimated that about 4 out of 5 persons already have gingivitis and 4 out of 10 have penodontitis
While good oral hygiene, as achieved by brushing the teeth with a cleansing dentifrice, may help reduce the incidence of periodontal disease, it does not necessarily prevent or eliminate its occurrence This is because microorganisms contribute to both the initiation and progress of periodontal disease Thus, in order to prevent or treat periodontal disease, these microorganisms must be suppressed by some means other than simple mechanical scrubbing Towards this end, there has been a great deal of research aimed at developing therapeutic dentifrices, mouthwashes, and methods of treating periodontal disease which are effective in suppressing these microorganisms
Dental calculus, or tartar as it is sometimes called, is a deposit which forms on the surfaces of the teeth at the gingival margin Supragingival calculus appears principally in the areas near the orifices of the salivary ducts; e g , on the lingual surfaces of the lower anterior teeth and on the buccal surfaces of the upper first and second molars, and on the distal surfaces of the posterior molars
Mature calculus consists of an inorganic portion which is largely calcium phosphate arranged in a hydroxyapatite crystal lattice structure similar to bone, enamel and dentine An organic portion is also present and consists of desquamated epithelial cells, leukocytes, salivary sediment, food debris and various types of microorganisms
As the mature calculus develops, it becomes visibly white or yellowish in color unless stained or discolored by some extraneous agent
A wide variety of chemical and biological agents have been suggested in the art to retard calculus formation or to remove calculus after it is formed Mechanical removal of this material periodically by the dentist is, of course, routine dental office procedure
The chemical approach to calculus inhibition generally involves chelation of calcium ions and/or crystal growth inhibition which prevents the calculus from forming and/or breaks down mature calculus by removing calcium
Tπclosan and herbal materials have been disclosed individually for use in oral products to combat plaque and gingivitis
Although there have been a number of approaches disclosed for combating periodontal disease, canes and calculus, there is still the desire and need to develop improved products possessing such properties
It is an object of the present invention to provide methods for obtaining extracts of golden thread and honeysuckle flowers and similar materials
These and other objects will become more clear from the detailed description which follows
All percentages and ratios used herein are by weight unless otherwise specified Also all measurements referred to herein are made at 25°C in the composition or on the pure matenal unless otherwise specified
SUMMARY OF THE INVENTION The present invention embraces a method of obtaining herbal extracts
DETAILED DESCRIPTION OF THE INVENTION
The compositions of the present invention comprise water insoluble noncationic and/or specific herbal extract materials obtained using the disclosed process
By "safe and effective amount" as used herein means sufficient amount of material to provide the desired benefit while being safe to the hard and soft tissues of the oral cavity
By the term "compnsing", as used herein, is meant that various additional components can be conjointly employed in the compositions of this invention as long as the listed materials perform their intended functions
By the term "acceptable earner", as used herein, is meant a suitable earner which can be used to apply the present agent(s) to the oral cavity without undue toxicity, irritation, allergic response and the like, commensurate with a reasonable benefit/risk ratio
Water Insoluble Noncationic Agents
Given below are examples of antibacterial agents useful in the compositions of the present invention which are water insoluble and noncationic.
Halogenated Diphenyl Ethers 2',4,4'-trichloro-2-hydroxy-diphenyl ether (Triclosan) 2,2'-dihydroxy-5,5'-dibromo-diphenyl ether.
Phenolic Compounds (including phenol and its homologs, mono- and poly-alkyl and aromatic halophenols, resorcinol and its derivatives, bisphenolic compounds and halogenated salicylanilides).
Phenol and its Homologs
Phenol
2 Methyl - Phenol
3 Methyl - Phenol
4 Methyl - Phenol
4 Ethyl - Phenol
2,4-Dimethyl - Phenol
2,5-Dimethyl - Phenol
3,4-Dimethyl - Phenol
2,6-Dimethyl - Phenol
4-n-Propyl - Phenol
4-n-Butyl - Phenol
4-n-Amyl - Phenol
4-tert-Amyl - Phenol
4-n-Hexyl - Phenol
4-n-Heptyl - Phenol
Mono- and Polv-Alkvl and Aromatic Halophenols p-Chlorophenol
Methyl- p-Chlorophenol
Ethyl - p-Chlorophenol n-Propyl - p-Chlorophenol n-Butyl - p-Chlorophenol n-Amyl - p-Chlorophenol sec- Amy 1 - p-Chlorophenol n-Hexyl - p-Chiorophenol
Cyclohexyl - p-Chlorophenol n-Hepty. - p-Chlorophenol n-Octyl - p-Chlorophenol
o-Chlorophenol
Methyl- o-Chlorophenol
Ethyl - o-Chlorophenol n-Propyl - o-Chlorophenol n-Butyl - o-Chlorophenol n-Amyl - o-Chlorophenol tert-Amyl ■ o-Chlorophenol n-Hexyl - o-Chlorophenol n-Heptyl ■ o-Chlorophenol o-Benzyl - p-Chlorophenol o-Benxyl-m-methyl - p-Chlorophenol o-Benzyl-m, m-dimethyl - p-Chlorophenol o-Phenylethyl - p-Chlorophenol o-Phenylethyl-m-methyl - p-Chlorophenol
3-Methyl - p-Chlorophenol
3,5-Dimethyl - p-Chlorophenol
6-Ethyl-3-methyl - p-Chlorophenol
6-n-Propyl-3-methyl - p-Chlorophenol
6-ιso-Propyl-3-methyl - p-Chlorophenol
2-Ethyl-3,5-dιmethyl - p-Chlorophenol
6-sec-Butyl-3-methyl - p-Chlorophenol
2-ιso-Propyl-3,5-dimethyl - p-Chlorophenol
6-Dιethylmethyl-3-methyl - p-Chlorophenol
6-ιso-Propyl-2-ethyl-3-methyl - p-Chlorophenol
2-sec-Amy 1-3, 5-d imethy I - p-Chlorophenol
2-Dιethylmethyl-3,5-dimethyl - p-Chlorophenol
6-sec-Octyl-3-methyl - p-Chlorophenol p-Bromophenol
Methyl - p-Bromophenol
Ethyl - p-Bromophenol n-Propyl - p-Bromophenol n-Butyl - p-Bromophenol n-Amyl - p-Bromophenol sec-Amyl - p-Bromophenol n-Hexyl - p-Bromophenol cyclohexyl - p-Bromophenol
o-Bromophenol tert-Amyl - o-Bromophenol n-Hexyl - o-Bromophenol n-Propyl-m,mDιmethyl - o-Bromophenol 2-Phenyl Phenol 4-Chloro-2-methyl phenol 4-Chloro-3-methyl phenol 4-Chloro-3,5-dιmethyl phenol 2,4-dιchloro-3,5-dιmethylphenol 3,4,5,6-terabromo-2-methylphenol 5-methyl-2-pentylphenol 4-ιsopropyl-3-methylphenol 5-Chloro-2-hydroxydιphenylmethane Resorcinol and its Derivatives
Resorcinol
Methyl - Resorcinol
Ethyl - Resorcinol n-Propyl - Resorcinol n-Butyl - Resorcinol n-Amyl - Resorcinol n-Hexyl - Resorcinol n-Heptyl - Resorcinol n-Octyl - Resorcinol n-Nonyl - Resorcinol
Phenyl - Resorcinol
Benzyl - Resorcinol
Phenylethyl - Resorcinol
Phenylpropyl - Resorcinol p-Chlorobenzyl - Resorcinol
5-Chloro -2,4-Dιhydroxydιphenyl Methane
4'-Chloro -2,4- -Dihydroxydiphenyl Methane
5-Bromo -2,4* -Dihydroxydiphenyl Methane
4'-Bromo -2,4- -Dihydroxydiphenyl Methane
Bisphenolic Compounds
2,2'-methylene bis (4-chlorophenol) 2,2'-methylene bis (3,4,6-trιchlorophenol)
2,2'-methylene bis (4-chloro-6-bromophenol) bis (2-hydroxy-3,5-dιchlorophenyl) sulphide bis (2-hydroxy-5-chlorobenzyl) sulphide
Halogenated Salicylanilides 4',5-dιbromosalιcyianιlιde 3,4',5-trιchlorosalcylanιiιde 3,4',5-trιbromosalιcylanιlιde 2,3,3',5-tetrachlorosalιcylanιlιde 3, 3', 5-tπchlorosalιcy lani de 3,5-dιbromo-3'-trιfiuoromethyl salicylanilide 5-n-octanoyl-3'-tπfluoromethyl salιcylanιlιde 3, 5-dιbromo-4'-trιfluoromethyl salicylanilide 3,5-dιbromo-3'-tnfluoromethyl salicylanilide
(Fluorophene)
Benzoic Esters p-Hydroxybenzoic Acid
Methyl - p-Hydroxybenzoic Acid
Ethyl - p-Hydroxybenzoic Acid
Propyl - p-Hydroxybenzoic Acid
Butyl - p-Hydroxybenzoic Acid
Halogenated Carbanilides 3,4 , 4'-trιch lorocarbanilide 3-tπfiuoromethyl-4,4'-dιchlorocarbanιlιde 3, 3' ,4-tπchlorocarbanιlιde
The water insoluble noncationic agent, when present, is present in the oral compositions of the present invention in an effective antiplaque amount, typically about 0 005-5% by weight, preferably about 0 005-1% The agent is substantially water-insoluble, meaning that its solubility is less than about 1% by weight in water at 25°C and may be even less than about 0 1% If an lonizable group is present solubility is determined at a pH at which lonization does not occur
Extracts of Golden Thread and Honeysuckle Flowers
The extracts of herbal materials useful in the development described and claimed herein are extracts of honeysuckle flowers, extracts of golden thread, or mixtures thereof One of the active agents in golden thread is berbenne A reference disclosing berbenne is U S 5,407,921 April 18, 1995, to Katsuragi et al incorporated herein by reference in its entirety Another patent disclosing berbenne is U S Patent 4,735,945, April 5, 1988, to Sakamoto et al also incorporated by reference herein in its entirety
Golden thread and honeysuckle flowers are natural materials and can be obtained from the plants themselves or the active components can be synthesized if desired A supplier of these herbal materials is East Earth Herb, Inc , Eugene, Oregon
An active component of golden thread, berbenne, and of honeysuckle flowers, chlorogenic acid, can be obtained from a number of different sources These for berbenne include the following
Many Herbs From Berbeπs, Nadina, Mahonia, Thalictrum spp and very many others in several different families (Annonaceae,
Berbendaceae, Menispermaceae, Papaveraceae, Ranunculaceae,
Rutaceae and Zingiberaceae) Honeysuckle flower substitutes include the following which are all mateπals which contain chlorogenic acid and/or luteo n flavonoids
Many Herbs from Capnoliaceae family and spp in many other families
(Leguminosae, Flacourtiaceae, Scrophulaπaceae, Euphorbiaceae,
Fabaceae, Asteraceae, Cistaceae, Passifloraceae, Heptaceae,
Juncaeae, Compositae, Resedaceae, Rubiaceae, Labiatae,
Umbelhferae, Logan laceae, Valeπanaceae, Menyanthaceae,
Cornaceae) Golden thread and honeysuckle flowers extracts are present in the products of this invention at an effective level, generally at a level of 0 005% to about 25% preferably from about 0 01% to about 10% most preferably of from about 3% to about 5%
Acceptable Carπer
The carrier for the active component(s) can be any vehicle suitable for use in the oral cavity Such carriers include the usual components of mouthwashes, toothpastes, tooth powders, prophylaxis pastes, lozenges, gums and the like and are more fully described hereinafter. Dentifrices and mouthwashes are the preferred systems.
In addition to the active agent(s), the present compositions may contain other antiplaque/gingivitis agents such as quaternary ammonium compounds, water, staπnous salts and zinc salts These types of agents are described in U.S Patent 4,656,031 , April 7, 1987 to Lane et al , and U S. Patent 5,004,597, April 2, 1991 to Majeti et al All incorporated herein by reference in their entirety
The abrasive polishing material contemplated for use in the present toothpaste part invention can be any material which does not excessively abrade dentin These include, for example, silicas including gels and precipitates, calcium carbonate, dicalcium orthophosphate dihydrate, calcium pyrophosphate, tπcalcium phosphate, calcium polymetaphosphate, insoluble
SUBSTITUTE 8liEET L£2B)
sodium polymetaphosphate, hydrated alumina, and resinous abrasive materials such as particulate condensation products of urea and formaldehyde, and other such as disclosed by Cooley et al in U S Patent 3,070,510, December 25, 1962, incorporated herein by reference Mixtures of abrasives may also be used
Silica dental abrasives, of various types, can provide the unique benefits of exceptional dental cleaning and polishing performance without unduly abrading tooth enamel or dentin Silica abrasive materials are also exceptionally compatible with sources of soluble fluoride and polyphosphonates For these reasons they are preferred for use herein
The silica abrasive polishing materials useful herein, as well as the other abrasives, generally have an average particle size ranging between about 0 1 to 30 microns, preferably 5 and 15 microns The silica abrasive can be precipitated silica or silica gels such as the silica xerogels described in Pader et al , U S Patent No 3,538,230, issued March 2, 1970 and DiGiu o, U S Patent No 3,862,307, June 21 , 1975, both incorporated herein by reference Preferred are the silica xerogels marketed under the tradename "Syloid" by the W R Grace & Company, Davison Chemical Division Preferred precipitated silica materials include those marketed by the J M Huber Corporation under the tradename, "Zeodent", particularly the silica carrying the designation "Zeodent 119" These silica abrasives are described in U S Patent No 4,340,583, July 29, 1982, incorporated herein by reference
The abrasive in the compositions described herein is present at a level of from about 6% to about 70%, preferably from about 15% to about 25% when the dentifrice is a toothpaste Higher levels, as high as 90%, may be used if the composition is a toothpowder
Flavoring agents can also be added to dentifrice compositions Suitable flavoring agents include oil of wintergreen, oil of peppermint, oil of spearmint, and oil of clove Sweetening agents which can be used include aspartame, acesulfame, saccharin, dextrose, levulose and sodium cyclamate Flavoring and sweetening agents are generally used in dentifrices at levels of from about 0 005% to about 2% by weight
Dentifrice compositions can also contain emulsifying agents Suitable emulsifying agents are those which are reasonably stable and foam throughout a wide pH range, including nonsoap anionic, noniontc, cationic, zwitteπonic and amphoteπc organic synthetic detergents Many of these suitable surfactants are disclosed by Gieske et al in U S Patent No 4,051 ,234, September 27, 1977, incorporated herein by reference
Water is also present in the toothpastes of this invention Water employed in the preparation of commercially suitable toothpastes should preferably be deionized and free of organic impurities Water generally comprises from about 10% to 50%, preferably from about 20% to 40%, by weight of the toothpaste compositions herein These amounts of water include
SUBSTITUTE SHEET (RULE 28)
the free water which is added plus that which is introduced with other materials such as with sorbitol
In preparing toothpastes, it is necessary to add some thickening material to provide a desirable consistency Preferred thickening agents are carboxyvinyl polymers of the type mentioned previously herein, xanthan gum, carrageenan, hydroxyethyl cellulose and water soluble salts of cellulose ethers such as sodium carboxymethyl cellulose and sodium carboxymethyl hydroxyethyl cellulose Natural gums such as gum karaya, gum arable, and gum tragacanth can also be used Colloidal magnesium aluminum silicate or finely divided silica can be used as part of the thickening agent to further improve texture Thickening agents in an amount from 0 10% to 5 0% by weight of the total composition can be used
It is also desirable to include some humectant matenal in a toothpaste to keep it from hardening Suitable humectants include glycerin, xylitol sorbitol, and other edible polyhydnc alcohols at a level of from about 5% to about 70%
Another preferred embodiment of the present invention is a mouthwash composition Conventional mouthwash composition components can compπse the carrier for the active agents of the present invention Mouthwashes generally comprise from about 20 1 to about 2 1 of a water/ethyl alcohol solution and preferably other ingredients such as flavor, sweeteners, humectants and sudsing agents such as those mentioned above for dentifrices The humectants give a moist feel to the mouth Generally, on a weight basis the mouthwashes of the invention comprise 0% to 60% (preferably 10% to 25%) ethyl alcohol, 0% to 20% (preferably 5% to 20%) of a humectant, 0% to 2% (preferably 0 01% to 0 15%) emulsifying agent, 0% to 0 5% (preferably 0 005% to 0 06%) sweetening agent such as saccharin, 0% to 0 3% (preferably 0 03% to 0 3%) flavoring agent, and the balance water
Suitable lozenge and chewing gum components are disclosed in U S Patent No 4,083,955, Apπl 11, 1978 to Grabenstetter et al , incorporated herein by reference in its entirety
Other optional components useful in the present invention are pyrophosphate salts such as those described in U S 4,515,772, May 7, 1985 to Parran et al incorporated herein by reference
Another agent which can be used in the present compositions is an alkali metal bicarbonate, such as sodium bicarbonate These are stable items of commerce and can be used together with a peroxide compound in separate compartments such as disclosed in U S 4,849,213 and U S 4,528,180, both to Schaeffer, incorporated herein by reference in their entirety
The pH of the present compositions and/or its pH in the mouth can be any pH which is safe for the mouth's hard and soft tissues Such pH's are generally from about 3 to about 10 preferably from about 4 to about 8 5
METHOD OF MANUFACTURE
The carrier compositions of the present invention can be made using methods which are common in the oral products area
For example, toothpaste compositions may be prepared by mixing part of the humectant and water together and heating to 660-71°C The fluoride source, if present, is then added along with the sweetener, the herbal materials are then added followed by the opacifier and the flavor
The herbal extracts useful in the present inventions are formed using the processes set forth below
Preparation of Crude Herbal Material for Extraction
1 Crude herbal materials are milled into fine powders
A Fitzmill comminuting mill is alternately used to a Retschmill for specific milling or reduced sizing needs (e g , coarse gπnding or cryogenic milling) Any grinding operation that achieves the respective particle size for extraction is acceptable
Crude herb extractibi ty is a critical function of exposed surface area of crude herb powder to water mass ratio To eliminate crude herb particle size as a process variable and since the various herbs have different water-holding capability (porosity/absorptivity), a singular particle size is preferred for process control
Depending on the specific type of crude herbs, milling produces a mix of coarse and fine dust particulates
2 All milled crude herb powders are mixed in a Ribbon-type blender for five to 120 minutes to provide uniform particle size of crude herbs prior to extraction
Particle size of milled crude herbal powder is consistent following this step Alternate blenders such as Waπng is acceptable Residual fines are discarded at this step Crude Herbal Matenal Extractions in Water (Either option is suitable)
3 a ) Soxhlet option
About 1-60 parts of milled crude herbal powder are added to 100-5000 parts (process and/or deionized or equivalent grade) water in a Soxhlet Extractor and then decanted A Soxhlet extractor is one or more station continuous reflux extractor with internal condenser slowly feeding 4-100°C water across the herb for up to 48 hours ) Ultrasonics option
Suitable alternate extraction process for developing this water soluble extract include use of ultrasonic water extraction systems which can provide equivalent quality, depending on the herb, with up to 94% faster process cycles Other suitable extraction processes include hydrolysis extracting reactors, fixed bed extracting reactors, desorption extraction columns,
SUBSTITUTE 8HEET (RULE 26)
and countercurrent extractors Due to most commercial extraction process limitations, it is normal to have a small amount of particulates in this extract The ratio of herbs to water used in the ultrasonic device is about 2 1 to about 320 1, the extraction temperature is from about 4°C to about 100°C, and the time of extraction is from about 30 minutes to 60 minutes
4 Water-extracted herbal liquid is filtered (e g , 5-100 μ filter cartridge, fine screen or cheesecloth) or centnfuged to remove coarse and/or insoluble particulates
5 Filtered water-extracted herbal liquid is concentrated, depending on herbal ingredient, up to a 50% soluble solids level
In addition to concentration by evaporation, alternate suitable process to achieve higher concentrations prior to final drying include freeze concentration, partial freeze drying, membrane separation, vacuum distillation and vacuum drying
6 Concentrated herbal extract liquids are dried via commercial drying processes
Suitable driers that are used include fluidized bed, freeze dπer, vacuum plate, spray, drum- type and flash driers Drying efficiency is controlled for water content (<10%) and free water considerations (<0 80) to achieve shelf-stability Yield of soluble powder from the drying process is used as key to optimize herb water mass formula for extraction
7 Dried pure solid herbal extract powders are sized and packaged for shipment A dessicating-mateπals such as a silica gel or other suitable FDA-approved, drying agent can be used to control relative humidity and to improve shelf-life
8 Dried pure solid herbal extract powder is now ready for reconstitution into oral care products
COMPOSITIONS USE The following examples further describe and demonstrate preferred compositions employing the process of the present invention The examples are given solely for illustration and are not to be construed as limitations of this invention as many vanations thereof are possible without departing from the spirit and scope thereof
EXAMPLE I
Given below is a composition representative of the present invention
Component Weight % Sodium Fluoπde, USP 0321 Sorbitol, LSR 32662 Silica, Precipitated 20000 RO Water 15478
Glyceπne, Synthetic 8000 Sodium Alkyl Sulfate Soln 7500 PEG 300 Carbowax, NF (PEG6) 6000 Tetrapotassium pyrophosphate (60% solution) 4212 Sodium acid pyrophosphate 1386 Tetrasodium Pyrophosphate Anhydrous 1353 Flavor 1000
Titanium Dioxide, USP (Rutile) 0525 Keltrol (Xanthan Gum, Food Grade) 0500 Sacchann 0470
Tnclosan 99% (irgacare MP) 0280 Carbopol 956 0250
Honeysuckle Flowers Extract, Pure Solid 0025 Golden Thread Extract, Pure Solid 0025 Pigment 0013
In the above compositions, the herbs may be varied using levels set forth herein before Additionally, the compositions may contain other antiplaque/antigingivitis or anticaries components, such as black tea, oolong tea, green tea, quaternary ammonium compounds, and metal salts such as stannous salts and zinc salts Furthermore, members of the Ericaceae family may be used Green, oolong, and black teas are members of the general tea family (Camillia Sinenis) and may also be used in the compositions of the present invention
Claims
WHAT IS CLAIMED IS
1 A method of herbal extraction comprising
(a) forming the crude herbal materials into the form of amilled herbal powder,
(b) forming a mixture of the milled herb powder and water,
(c) exposing the mixture of (b) to an ultrasonic water extraction system, and
(d) drying of extract to a water activity of < 0 80
2 The method of Claim 1 wherein the herbal materials extracted are selected from the group consisting of golden thread, honeysuckle flowers and mixtures thereof
The method of either Claims 1 or 2 wherein the ratio of herb to water used in the ultrasonic extraction is from about 2 1 to about 320 1
4 The method of any of Claims 1 -3 wherein the extraction temperature is from about 4°C to about 182°C
5 The method of any of Claims 1-4 wherein the time of extraction is from about 5 to about 120 minutes
6 An oral composition containing a herbal extract produced according to Claim 1
7 A composition according to Claim 6 which in addition contains water-insoluble noncationic antibacterial agents
8 A composition according to either Claims 6 or 7 wherein the herbal extract is berbenne
9 A composition according to any of Claims 6-8 wherein extracts of honeysuckle flowers and golden thread are added at 0 005% to 5%
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US69549096A | 1996-08-12 | 1996-08-12 | |
US08/695,490 | 1996-08-12 |
Publications (1)
Publication Number | Publication Date |
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WO1998006377A1 true WO1998006377A1 (en) | 1998-02-19 |
Family
ID=24793211
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US1997/013042 WO1998006377A1 (en) | 1996-08-12 | 1997-08-06 | Oral compositions |
Country Status (1)
Country | Link |
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WO (1) | WO1998006377A1 (en) |
Cited By (4)
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EP0917825A3 (en) * | 1997-11-19 | 2000-06-28 | Akira Horigane | Frozen or freeze-dried product, process and apparatus for producing the same |
WO2002091848A1 (en) * | 2001-05-15 | 2002-11-21 | The Procter & Gamble Company | Confectionery compositions |
FR2825936A1 (en) * | 2001-06-18 | 2002-12-20 | Malemba Jean Claude Mapangou | Method of obtaining natural surfactants for use in detergents by extraction from the pulp of the strychnos gratus fruit |
US6706256B2 (en) | 2001-05-15 | 2004-03-16 | The Procter & Gamble Co. | Oral care compositions |
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EP0917825A3 (en) * | 1997-11-19 | 2000-06-28 | Akira Horigane | Frozen or freeze-dried product, process and apparatus for producing the same |
WO2002091848A1 (en) * | 2001-05-15 | 2002-11-21 | The Procter & Gamble Company | Confectionery compositions |
US6703000B2 (en) | 2001-05-15 | 2004-03-09 | The Procter & Gamble Co. | Confectionery compositions |
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