WO2022172790A1 - 化粧料 - Google Patents
化粧料 Download PDFInfo
- Publication number
- WO2022172790A1 WO2022172790A1 PCT/JP2022/003408 JP2022003408W WO2022172790A1 WO 2022172790 A1 WO2022172790 A1 WO 2022172790A1 JP 2022003408 W JP2022003408 W JP 2022003408W WO 2022172790 A1 WO2022172790 A1 WO 2022172790A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- acid
- hyaluronic acid
- agent
- salt
- mass
- Prior art date
Links
- 239000002537 cosmetic Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title abstract description 7
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 claims abstract description 253
- 229920002674 hyaluronan Polymers 0.000 claims abstract description 252
- 229960003160 hyaluronic acid Drugs 0.000 claims abstract description 252
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 105
- 150000003839 salts Chemical class 0.000 claims abstract description 85
- 239000002738 chelating agent Substances 0.000 claims abstract description 67
- -1 organic acid salts Chemical class 0.000 claims abstract description 16
- 230000008961 swelling Effects 0.000 claims abstract description 8
- 210000004209 hair Anatomy 0.000 claims description 47
- 238000000034 method Methods 0.000 claims description 29
- 150000001768 cations Chemical class 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 12
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 claims description 10
- 229960003330 pentetic acid Drugs 0.000 claims description 10
- 229910021645 metal ion Inorganic materials 0.000 claims description 9
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 9
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 9
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 9
- JYXGIOKAKDAARW-UHFFFAOYSA-N N-(2-hydroxyethyl)iminodiacetic acid Chemical compound OCCN(CC(O)=O)CC(O)=O JYXGIOKAKDAARW-UHFFFAOYSA-N 0.000 claims description 7
- WYMDDFRYORANCC-UHFFFAOYSA-N 2-[[3-[bis(carboxymethyl)amino]-2-hydroxypropyl]-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)CN(CC(O)=O)CC(O)=O WYMDDFRYORANCC-UHFFFAOYSA-N 0.000 claims description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical group OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 6
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 claims description 6
- RUSUZAGBORAKPY-UHFFFAOYSA-N acetic acid;n'-[2-(2-aminoethylamino)ethyl]ethane-1,2-diamine Chemical compound CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.NCCNCCNCCN RUSUZAGBORAKPY-UHFFFAOYSA-N 0.000 claims description 6
- WPPVJSFNBNUTHQ-UHFFFAOYSA-H hexasodium N'-[2-(2-aminoethylamino)ethyl]ethane-1,2-diamine hexaacetate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.NCCNCCNCCN WPPVJSFNBNUTHQ-UHFFFAOYSA-H 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 claims description 4
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 4
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 4
- 230000003796 beauty Effects 0.000 claims description 4
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 4
- 229940068041 phytic acid Drugs 0.000 claims description 4
- 235000002949 phytic acid Nutrition 0.000 claims description 4
- 239000000467 phytic acid Substances 0.000 claims description 4
- DIWZKTYQKVKILN-VKHMYHEASA-N (2s)-2-(dicarboxymethylamino)pentanedioic acid Chemical compound OC(=O)CC[C@@H](C(O)=O)NC(C(O)=O)C(O)=O DIWZKTYQKVKILN-VKHMYHEASA-N 0.000 claims description 3
- VKZRWSNIWNFCIQ-WDSKDSINSA-N (2s)-2-[2-[[(1s)-1,2-dicarboxyethyl]amino]ethylamino]butanedioic acid Chemical compound OC(=O)C[C@@H](C(O)=O)NCCN[C@H](C(O)=O)CC(O)=O VKZRWSNIWNFCIQ-WDSKDSINSA-N 0.000 claims description 3
- PQHYOGIRXOKOEJ-UHFFFAOYSA-N 2-(1,2-dicarboxyethylamino)butanedioic acid Chemical compound OC(=O)CC(C(O)=O)NC(C(O)=O)CC(O)=O PQHYOGIRXOKOEJ-UHFFFAOYSA-N 0.000 claims description 3
- JPGSFSFMINKKJZ-UHFFFAOYSA-N 2-[1,2-dicarboxyethyl(hydroxy)amino]butanedioic acid Chemical compound OC(=O)CC(C(O)=O)N(O)C(CC(O)=O)C(O)=O JPGSFSFMINKKJZ-UHFFFAOYSA-N 0.000 claims description 3
- DMQQXDPCRUGSQB-UHFFFAOYSA-N 2-[3-[bis(carboxymethyl)amino]propyl-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)CCCN(CC(O)=O)CC(O)=O DMQQXDPCRUGSQB-UHFFFAOYSA-N 0.000 claims description 3
- 229940120146 EDTMP Drugs 0.000 claims description 3
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 3
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims description 3
- FSVCELGFZIQNCK-UHFFFAOYSA-N N,N-bis(2-hydroxyethyl)glycine Chemical compound OCCN(CCO)CC(O)=O FSVCELGFZIQNCK-UHFFFAOYSA-N 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims description 3
- JKCPAFFNQYZVSE-NRXHRRLXSA-J [Na+].[Na+].[Na+].[Na+].C(CN([C@@H](CC(=O)[O-])C(=O)[O-])CC(=O)O)(=O)O.N([C@@H](CC(=O)[O-])C(=O)[O-])(CC(=O)O)CC(=O)O Chemical compound [Na+].[Na+].[Na+].[Na+].C(CN([C@@H](CC(=O)[O-])C(=O)[O-])CC(=O)O)(=O)O.N([C@@H](CC(=O)[O-])C(=O)[O-])(CC(=O)O)CC(=O)O JKCPAFFNQYZVSE-NRXHRRLXSA-J 0.000 claims description 3
- MLDWGLQSBBCMMO-UHFFFAOYSA-N [Na].[Na].[Na].CNCC(=O)O Chemical compound [Na].[Na].[Na].CNCC(=O)O MLDWGLQSBBCMMO-UHFFFAOYSA-N 0.000 claims description 3
- BTKOPDXMVKYSNL-UHFFFAOYSA-N [Na].[Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O Chemical compound [Na].[Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BTKOPDXMVKYSNL-UHFFFAOYSA-N 0.000 claims description 3
- PDIZYYQQWUOPPK-UHFFFAOYSA-N acetic acid;2-(methylamino)acetic acid Chemical compound CC(O)=O.CC(O)=O.CNCC(O)=O PDIZYYQQWUOPPK-UHFFFAOYSA-N 0.000 claims description 3
- WDJHALXBUFZDSR-UHFFFAOYSA-N acetoacetic acid Chemical compound CC(=O)CC(O)=O WDJHALXBUFZDSR-UHFFFAOYSA-N 0.000 claims description 3
- KYQODXQIAJFKPH-UHFFFAOYSA-N diazanium;2-[2-[bis(carboxymethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [NH4+].[NH4+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O KYQODXQIAJFKPH-UHFFFAOYSA-N 0.000 claims description 3
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 claims description 3
- DEFVIWRASFVYLL-UHFFFAOYSA-N ethylene glycol bis(2-aminoethyl)tetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)CCOCCOCCN(CC(O)=O)CC(O)=O DEFVIWRASFVYLL-UHFFFAOYSA-N 0.000 claims description 3
- 239000004220 glutamic acid Substances 0.000 claims description 3
- 235000013922 glutamic acid Nutrition 0.000 claims description 3
- LQPLDXQVILYOOL-UHFFFAOYSA-I pentasodium;2-[bis[2-[bis(carboxylatomethyl)amino]ethyl]amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC(=O)[O-])CCN(CC([O-])=O)CC([O-])=O LQPLDXQVILYOOL-UHFFFAOYSA-I 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- DZCAZXAJPZCSCU-UHFFFAOYSA-K sodium nitrilotriacetate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CC([O-])=O DZCAZXAJPZCSCU-UHFFFAOYSA-K 0.000 claims description 3
- DRKXDZADBRTYAT-DLCHEQPYSA-J tetrasodium (2S)-2-[bis(carboxymethyl)amino]pentanedioate Chemical compound C(=O)(O)CN([C@@H](CCC(=O)[O-])C(=O)[O-])CC(=O)O.[Na+].[Na+].[Na+].[Na+].C(=O)(O)CN([C@@H](CCC(=O)[O-])C(=O)[O-])CC(=O)O DRKXDZADBRTYAT-DLCHEQPYSA-J 0.000 claims description 3
- 229940080258 tetrasodium iminodisuccinate Drugs 0.000 claims description 3
- GYBINGQBXROMRS-UHFFFAOYSA-J tetrasodium;2-(1,2-dicarboxylatoethylamino)butanedioate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CC(C([O-])=O)NC(C([O-])=O)CC([O-])=O GYBINGQBXROMRS-UHFFFAOYSA-J 0.000 claims description 3
- 229940048081 trisodium ethylenediamine disuccinate Drugs 0.000 claims description 3
- QEHXDDFROMGLSP-VDBFCSKJSA-K trisodium;(2s)-2-[2-[[(1s)-1-carboxy-2-carboxylatoethyl]amino]ethylamino]butanedioate Chemical compound [Na+].[Na+].[Na+].OC(=O)C[C@@H](C([O-])=O)NCCN[C@H](C([O-])=O)CC([O-])=O QEHXDDFROMGLSP-VDBFCSKJSA-K 0.000 claims description 3
- IIFGCAJBLSOVSP-UHFFFAOYSA-N OCCN(CC(=O)O)CC(=O)O.[Na].[Na] Chemical compound OCCN(CC(=O)O)CC(=O)O.[Na].[Na] IIFGCAJBLSOVSP-UHFFFAOYSA-N 0.000 claims description 2
- PCBPAXFCVWQFRN-MJYQEAFUSA-J [Na+].[Na+].[Na+].[Na+].OC(=O)C(C(O)=O)N[C@H](C([O-])=O)CCC([O-])=O.OC(=O)C(C(O)=O)N[C@H](C([O-])=O)CCC([O-])=O Chemical compound [Na+].[Na+].[Na+].[Na+].OC(=O)C(C(O)=O)N[C@H](C([O-])=O)CCC([O-])=O.OC(=O)C(C(O)=O)N[C@H](C([O-])=O)CCC([O-])=O PCBPAXFCVWQFRN-MJYQEAFUSA-J 0.000 claims description 2
- DXGKKTKNDBFWLL-UHFFFAOYSA-N azane;2-[bis(carboxymethyl)amino]acetic acid Chemical compound N.N.N.OC(=O)CN(CC(O)=O)CC(O)=O DXGKKTKNDBFWLL-UHFFFAOYSA-N 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 21
- 230000003472 neutralizing effect Effects 0.000 abstract description 4
- 239000003906 humectant Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 121
- 235000002639 sodium chloride Nutrition 0.000 description 105
- 210000003491 skin Anatomy 0.000 description 65
- 239000000203 mixture Substances 0.000 description 56
- 238000012360 testing method Methods 0.000 description 53
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 38
- 230000003020 moisturizing effect Effects 0.000 description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 30
- 230000000694 effects Effects 0.000 description 25
- 239000011780 sodium chloride Substances 0.000 description 19
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 16
- 238000011156 evaluation Methods 0.000 description 14
- 239000012736 aqueous medium Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- 230000036961 partial effect Effects 0.000 description 11
- 239000000872 buffer Substances 0.000 description 10
- 239000001257 hydrogen Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- 239000007853 buffer solution Substances 0.000 description 8
- 239000004202 carbamide Substances 0.000 description 8
- 229940005740 hexametaphosphate Drugs 0.000 description 8
- 210000000434 stratum corneum Anatomy 0.000 description 8
- 238000002296 dynamic light scattering Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 239000004615 ingredient Substances 0.000 description 6
- 239000001509 sodium citrate Substances 0.000 description 6
- 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 6
- 229910001415 sodium ion Inorganic materials 0.000 description 6
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 239000007979 citrate buffer Substances 0.000 description 4
- 235000015165 citric acid Nutrition 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 230000036571 hydration Effects 0.000 description 4
- 238000006703 hydration reaction Methods 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 230000036548 skin texture Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 3
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 3
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Natural products OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 3
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 description 3
- 206010044625 Trichorrhexis Diseases 0.000 description 3
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 description 3
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
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- 239000000344 soap Substances 0.000 description 3
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- 238000003756 stirring Methods 0.000 description 3
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- 238000005406 washing Methods 0.000 description 3
- 102000011782 Keratins Human genes 0.000 description 2
- 108010076876 Keratins Proteins 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 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
- 239000012153 distilled water Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 229940071106 ethylenediaminetetraacetate Drugs 0.000 description 2
- 210000004709 eyebrow Anatomy 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- 229910001425 magnesium ion Inorganic materials 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N malic acid Chemical compound OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- 229940095064 tartrate Drugs 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
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- DCCWEYXHEXDZQW-BYPYZUCNSA-N (2s)-2-[bis(carboxymethyl)amino]butanedioic acid Chemical compound OC(=O)C[C@@H](C(O)=O)N(CC(O)=O)CC(O)=O DCCWEYXHEXDZQW-BYPYZUCNSA-N 0.000 description 1
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- QPTMDBQLCWRDCK-UHFFFAOYSA-I pentasodium;[2-[bis[[hydroxy(oxido)phosphoryl]methyl]amino]ethyl-(phosphonatomethyl)amino]methyl-hydroxyphosphinate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].OP([O-])(=O)CN(CP(O)([O-])=O)CCN(CP(O)([O-])=O)CP([O-])([O-])=O QPTMDBQLCWRDCK-UHFFFAOYSA-I 0.000 description 1
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- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
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Images
Classifications
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0241—Containing particulates characterized by their shape and/or structure
- A61K8/0245—Specific shapes or structures not provided for by any of the groups of A61K8/0241
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- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
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Definitions
- This disclosure relates to cosmetics.
- hyaluronic acid which has a moisturizing function, is used in fields such as cosmetics to moisturize the skin.
- Patent Document 1 includes hyaluronic acid-supporting nanoparticles in which hyaluronic acid is supported on at least one of the inside or surface of nanoparticles formed of polylactic acid, polyglycolic acid, or lactic acid/glycolic acid copolymer. , cosmetics are disclosed.
- Patent Document 2 discloses an external preparation for skin containing composite nanoparticles containing (A) hyaluronic acid and (B) a zwitterionic compound and having a particle size of 100 nm or less.
- Unpublished Patent Document 3 discloses a cosmetic containing an aqueous medium and hyaluronic acid particles dispersed in the aqueous medium, and wherein the average particle size of the hyaluronic acid particles is 200 nm or less.
- JP 2010-150151 A WO2018/182003 PCT/JP2020/031318
- Hyaluronic acid has a negative charge due to the presence of carboxyl groups. Due to the electrostatic repulsion based on this negative charge, hyaluronic acid generally spreads like a thread.
- Compacted hyaluronic acid tends to remain in, for example, skin crevices or pores, compared to hyaluronic acid that spreads like threads.
- the content of hyaluronic acid in the particles described in Patent Document 1 is as low as about 3% by mass, and the content of hyaluronic acid in the particles described in Patent Document 2 is only 50% by mass or less. In some cases, it was not possible to ensure the moisture retention.
- Patent Document 3 The researchers of the present applicant, as described in Patent Document 3, use the electrostatic shielding effect of an electrolyte such as sodium chloride to apparently neutralize the negative charge based on the carboxyl group of hyaluronic acid, attracting The present inventors have found that by making the hydrogen bonds based on the hydroxyl groups in hyaluronic acid that exert their effects dominant, the spreading of hyaluronic acid can be suppressed and the hyaluronic acid can be made compact.
- an electrolyte such as sodium chloride
- the subject of the present disclosure is to provide a cosmetic that can ensure sufficient moisturizing properties even when compacted hyaluronic acid is used by neutralizing the carboxyl groups of hyaluronic acid with a salt. is.
- the chelating agent is ethylenediaminetetraacetic acid, disodium ethylenediaminetetraacetic acid, trisodium ethylenediaminetetraacetic acid, nitrilotriacetic acid, sodium nitrilotriacetate, ammonium nitrilotriacetate, hydroxyethylethylenediaminetriacetic acid, sodium hydroxyethylethylenediaminetriacetate, pentetic acid.
- pentasodium pentetate triethylenetetramine hexaacetic acid, sodium triethylenetetramine hexaacetate, imidisuccinic acid, tetrasodium imidisuccinate, ethylenediaminedisuccinic acid, trisodium ethylenediaminedisuccinate, hydroxyethyliminodiacetic acid, hydroxyethyliminodiacetic acid Disodium, iminodisuccinic acid, tetrasodium iminodisuccinate, triethylenetetramine hexaacetic acid, sodium triethylenetetramine hexaacetate, methylglycine diacetate, trisodium methylglycine diacetate, hydroxyiminodisuccinic acid, hydroxyiminodisuccinate tetrasodium L-aspartic acid, tetrasodium L-aspartic acid diacetate, glutamic acid diacetic acid,
- 1 is a graph showing the substance amount (mol) of a chelating agent (HMP) with respect to 100 mol of salt (MgCl 2 ) and the expandability of compacted hyaluronic acid. It is a graph regarding the substance amount (mol) of a chelating agent (HMP) with respect to 100 mol of salt (NaCl) and the swelling property of compacted hyaluronic acid.
- 1 is a graph showing changes in stratum corneum water content before and after application of various test samples to the skin.
- 1 is a graph showing changes in skin texture number before and after application of various test samples to the skin.
- 4 is a graph of Z-average particle size and ionic strength of hyaluronic acid particles prepared using sodium chloride.
- 4 is a graph showing the Z-average particle size and ionic strength of hyaluronic acid particles in compositions with different hyaluronic acid concentrations prepared using sodium chloride.
- 4 is a graph showing the Z-average particle size and ionic strength of hyaluronic acid particles in compositions with hyaluronic acid concentrations of 0.4 mass % and 0.5 mass % prepared using sodium chloride. It is a graph regarding the Z-average particle size and moisturizing performance of hyaluronic acid particles.
- 4 is a graph relating to Z-average particle size and ionic strength of hyaluronic acid particles prepared using a citrate buffer.
- 4 is a graph relating to the Z-average particle size of hyaluronic acid particles with the addition of urea.
- the cosmetic of the present disclosure includes a first agent containing at least one salt selected from the group consisting of inorganic salts and organic acid salts, and hyaluronic acid, and a second agent for swelling hyaluronic acid, which contains a chelating agent. and
- Hyaluronic acid generally has a negative charge due to the presence of carboxyl groups. Due to the electrostatic repulsion based on this negative charge, for example, hyaluronic acid molecules tend to spread like threads and tend to be difficult to compact. For this reason, in order to shrink the structure of hyaluronic acid molecules and make them compact, a nanometer-order supporting material capable of supporting hyaluronic acid molecules was required, as in Patent Documents 1 and 2. As a result, restrictions have been imposed on the content of hyaluronic acid in compacted structures.
- the negative charge of hyaluronic acid is apparently neutralized by utilizing the electrostatic shielding effect of an electrolyte such as sodium chloride, and the hydrogen bond is dominant, so that the hyaluronic acid molecule It is possible to suppress the spread of the hyaluronic acid molecule and make it compact even if it is a single hyaluronic acid molecule. Since the compacted hyaluronic acid structure prepared by the technique of Patent Document 3 can be prepared without using a support material as described above, the content of hyaluronic acid in such a structure can be theoretically It can be 100% by mass.
- the cosmetic of the present disclosure comprises a second agent containing a chelating agent. Since such a second agent can capture components that neutralize the negative charge of the carboxyl group (for example, metal ions such as sodium ions), hyaluronic acid compacted using salt is applied to the skin or body hair. It is believed that if a second agent containing a chelating agent is applied after this, cations such as sodium ions that have neutralized the carboxyl groups can be captured. As a result, the carboxyl groups in hyaluronic acid can sufficiently express the ability to hold water (hydration ability), so that it is possible to provide good moisturizing properties to the skin or body hair. thinking.
- a second agent containing a chelating agent can capture components that neutralize the negative charge of the carboxyl group (for example, metal ions such as sodium ions), hyaluronic acid compacted using salt is applied to the skin or body hair. It is believed that if a second agent containing a chelating agent is applied
- FIGS. When a chelating agent is blended in a solution containing hyaluronic acid that has been compacted using a salt, the compacted hyaluronic acid swells. In other words, it is considered that such a swelling phenomenon occurs as a result of the cations such as sodium ions being captured by the addition of the chelating agent and the electrostatic shielding effect being reduced.
- the chelating agent itself also contains metal ions, the hyaluronic acid can become compact again when the amount of the chelating agent increases.
- the optimum amount of the chelating agent varies depending on the type of the chelating agent, but if the chelating agent is blended in the second agent so as to swell the hyaluronic acid compacted with salt, the cosmetic of the present disclosure will eventually become can provide good moisturizing properties.
- Hyaluronic acid compacted with salt can also be swollen with urea, as shown in FIG.
- swelling with urea is not obtained by reducing the electrostatic shielding effect, but is obtained by breaking hydrogen bonds resulting from compaction.
- the cosmetic of the present disclosure includes a first agent and a second agent.
- the first agent of the present disclosure contains at least one salt selected from the group consisting of inorganic salts and organic acid salts, and hyaluronic acid.
- the salt that can be blended in the first agent of the present disclosure is not particularly limited as long as it can apparently neutralize the negative charge of hyaluronic acid.
- examples of such salts include at least one salt selected from inorganic salts and organic acid salts.
- inorganic salts and organic acid salts salts that hardly have an adverse effect on the skin or body hair are preferred.
- inorganic salt means a salt composed only of inorganic components, and can also be rephrased as a salt composed of ions generated from an inorganic acid and an inorganic base.
- organic acid salt means a salt formed by combining an organic acid and a metal ion.
- the salt generally exists in the form of salt-derived ions in the first agent. Therefore, in the present disclosure, for example, a “first agent containing a salt” is intended to include such salts in the form of ions. Also, ionic surfactants are not included in the "salts" of the present disclosure.
- Inorganic salts include, for example, sodium nitrate, sodium sulfate, sodium chloride, potassium nitrate, potassium sulfate, potassium chloride, calcium nitrate, calcium sulfate, calcium chloride, magnesium nitrate, magnesium sulfate, magnesium chloride, aluminum nitrate, aluminum sulfate, and chloride. Aluminum may be mentioned. These salts can be used individually or in combination of 2 or more types.
- organic acid salts include citrate, acetate, lactate, tartrate, succinate, malate, glycolate, salicylate, and pyrrolidone carboxylate.
- organic acids such as citric acid, acetic acid, lactic acid, tartaric acid, succinic acid, malic acid, glycolic acid, salicylic acid, and pyrrolidone carboxylic acid, and sodium ions, potassium ions, calcium ions, magnesium ions, aluminum ions, etc. Salts combined with metal ions can be mentioned. These salts can be used individually or in combination of 2 or more types.
- the cations constituting the salt are preferably metal ions, more preferably divalent or higher metal ions.
- the amount of salt compounded in the first agent may be appropriately selected according to the degree of compactness of hyaluronic acid, and there is no particular limitation.
- a compounding amount is, for example, 0.10% by mass or more, 0.20% by mass or more, 0.30% by mass or more, 0.40% by mass or more, or 0.50% by mass or more with respect to the total amount of the first agent. 5.0% by mass or less, 4.0% by mass or less, 3.0% by mass or less, 2.0% by mass or less, 1.9% by mass or less, 1.8% by mass or less, It can be 1.7% by mass or less, 1.6% by mass or less, or 1.5% by mass or less.
- the amount of salt in the first agent can also be defined as the ionic strength of the salt.
- the ionic strength of the salt can be, for example, 0.01 or more, 0.03 or more, or 0.05 or more, and 5.0 or less, 4.0 or less, 3.0 or less, 2.0 or less, or 1.0 or less.
- the amount or ionic strength of the salt depends on the salt component contained in the buffer solution itself and the amount added separately to the buffer solution. The calculation is based on all salt components, including salt components.
- Hyaluronic acid that can be blended in the first agent of the present disclosure is not particularly limited.
- hyaluronic acid means a linear polymer in which N-acetyl-D-glucosamine residues and D-glucuronic acid residues are alternately linked, and such hyaluronic acid is used, for example, in chicken combs or other animals. It can be obtained by isolation extraction from tissues or by fermentation using microorganisms such as Streptococcus.
- Hyaluronic acid may be a derivative thereof.
- derivatives of hyaluronic acid include hyaluronic acid metal salts such as hyaluronic acid sodium salt, hyaluronic acid potassium salt, hyaluronic acid magnesium salt, hyaluronic acid calcium salt, and hyaluronic acid aluminum salt.
- hyaluronic acid derivatives obtained by etherifying, esterifying, amidating, acetylating, acetalizing, or ketalizing the hydroxyl group, carboxyl group, etc. of hyaluronic acid.
- "hyaluronic acid” in the present disclosure may include the concept of hyaluronic acid and derivatives thereof.
- the weight average molecular weight of hyaluronic acid is not particularly limited, and can be, for example, 10,000,000 or less. From the viewpoint of water retention performance of hyaluronic acid and compactness of hyaluronic acid, the weight average molecular weight of hyaluronic acid is, for example, 500 or more, 1,000 or more, 5,000 or more, 10,000 or more, 50,000. 100,000 or more, 300,000 or more, 500,000 or more, 800,000 or more, or 1,000,000 or more, and 10,000,000 or less, 8,000,000 or less , 5,000,000 or less, 3,000,000 or less, 2,000,000 or less, or 1,500,000 or less.
- the weight average molecular weight intends the weight average molecular weight in terms of polystyrene in gel permeation chromatography measurement.
- the hyaluronic acid of the present disclosure can take the form of particles with an average particle size of 200 nm or less.
- Hyaluronic acid in such a form can easily penetrate into the skin or body hair, for example, it can penetrate into the skin non-invasively through the stratum corneum or pores of the skin.
- relatively low-molecular-weight hyaluronic acid with a weight-average molecular weight of less than 500 is considered to easily penetrate skin or body hair without microparticulation.
- such low-molecular-weight hyaluronic acid is less likely to remain in the skin or body hair, and is inferior in water retention performance to high-molecular-weight hyaluronic acid. can be difficult.
- the hyaluronic acid particles of the present disclosure can be prepared using hyaluronic acid having a weight average molecular weight of 500 or more, and such hyaluronic acid can be highly contained in the particles.
- the obtained hyaluronic acid particles are likely to stay inside the skin or body hair, and can maintain the moisturizing effect inside the skin or body hair for a long period of time.
- hyaluronic acid and its derivatives can be used alone or in combination of two or more. Moreover, the molecular weights of the hyaluronic acid and its derivatives used may be the same or different.
- a commercially available product may be used for hyaluronic acid.
- hyaluronic acid examples include hyaluronic acid HA-LQ (manufactured by Kewpie Co., Ltd.), hyaluronic acid FCH (manufactured by Kikkoman Biochemifa Corporation), and biosodium hyaluronate HA12N (manufactured by Shiseido Co., Ltd.).
- the hyaluronic acid contained in the first agent of the present disclosure shrinks due to the electrostatic shielding effect based on the salt and the action of hydrogen bonding, and the hyaluronic acid molecule is in a form such that it is singly or multiple entangled and aggregated (this form may be referred to as “hyaluronic acid aggregate shrinkage”). Since such a form of hyaluronic acid can be prepared without using a supporting material as described in Patent Documents 1 and 2, the content ratio of hyaluronic acid in the hyaluronic acid aggregate shrinkage product can be theoretically It can be 100% by mass. That is, the hyaluronic acid aggregate and shrinkage product of the present disclosure can be composed of hyaluronic acid molecules alone as the polymer component.
- the hyaluronic acid aggregate and shrinkage product of the present disclosure may contain polymer components other than hyaluronic acid within a range that does not cause problems such as moisturizing performance.
- the content of other polymer components is, for example, 20% by mass or less, 10% by mass or less, 5% by mass or less, 3% by mass or less, or 1% by mass with respect to the total amount of polymer contained in the hyaluronic acid aggregated shrinkage product. % or less.
- hyaluronic acid aggregated shrinkage product can be intended to include a high degree of hyaluronic acid component, and the proportion of hyaluronic acid component as described in Patent Documents 1 and 2 Particles with a content of 50% by mass or less are not included.
- the content of hyaluronic acid in the hyaluronic acid-aggregated shrinkage product can be measured using, for example, the ELISA method.
- the hyaluronic acid aggregate shrinkage product has a thread-like particle form measurable by a dynamic light scattering method (this form is further referred to as "hyaluronic acid may be referred to as "particles").
- hyaluronic acid may be referred to as "particles"
- the penetration of hyaluronic acid particles into the skin or body hair varies from person to person, and may vary depending on the condition of the stratum corneum, the condition of hair, the number or size of pores, etc. However, particles with an average particle size of 200 nm or less , the particles can penetrate most skin or hair.
- the average particle size of hyaluronic acid particles can be, for example, 150 nm or less, 120 nm or less, or 100 nm or less. Above, it can be 30 nm or more, or 50 nm or more.
- the average particle size means the Z-average particle size of hyaluronic acid particles optically measured by a dynamic light scattering method, assuming that the particle shape of the hyaluronic acid particles is spherical.
- Such average particle size can be measured using, for example, Zetasizer (manufactured by Malvern Panalytical) or dynamic light scattering photometer DLS-8000 (manufactured by Otsuka Electronics). These measurement devices can be appropriately selected based on the overlap concentration of each hyaluronic acid. For example, below overlap concentration, a dynamic light scattering photometer DLS-8000 can be used, and above overlap concentration, a Zetasizer can be used. Overlap concentration can be calculated, for example, by confocal post-bleaching fluorescence recovery method (Confocal-FRAP).
- Confocal-FRAP confocal post-bleaching fluorescence recovery method
- Hyaluronic acid particles with an average particle size of 200 nm or less can penetrate into the skin or body hair, but because the particle size is small, it is considered difficult to stay inside the skin or body hair.
- a second agent containing a chelating agent can be applied to such hyaluronic acid particles to swell the particles. That is, after the hyaluronic acid has penetrated into the skin or body hair, the second agent can be applied to swell the hyaluronic acid inside the skin or body hair, so that the hyaluronic acid can be retained inside the skin or body hair. can. As a result, the moisturizing effect inside the skin or body hair can be sustained for a longer period of time.
- the content of hyaluronic acid in the first agent is, for example, 0.005% by mass or more, 0.01% by mass or more, and 0.05% by mass relative to the total amount of the first agent from the viewpoint of moisture retention, cost, etc. % or more, 0.10 mass % or more, 0.15 mass % or more, 0.20 mass % or more, or 0.25 mass % or more, and 1.0 mass % or less, 0.80 mass % % or less, 0.60 mass % or less, 0.50 mass % or less, or 0.45 mass % or less.
- the hyaluronic acid contained in the first agent of the present disclosure has a high content of hyaluronic acid in the hyaluronic acid aggregated shrinkage product, and due to the action of the chelating agent of the second agent, the hyaluronic acid Since the hydration ability based on the carboxyl group is excellent, sufficient moisturizing effect can be exhibited even when the content of hyaluronic acid in the first agent is relatively low.
- the first agent of the present disclosure may typically contain an aqueous medium.
- an aqueous medium is not particularly limited, and an aqueous medium used for cosmetics, quasi-drugs, etc. can be used.
- ion-exchanged water, distilled water, ultrapure water, tap water, buffer solution, etc. can be used.
- An aqueous medium can be used individually or in combination of 2 or more types.
- buffers include citrate buffer, lactate buffer, phosphate buffer, acetate buffer, tartrate buffer, borate buffer, and Tris buffer. From the viewpoint of high buffer capacity, citrate buffer, lactate buffer and phosphate buffer are preferred, and citrate buffer is more preferred.
- the pH of the buffer solution can be 7.0 or less, 6.8 or less, or 6.5 or less.
- the lower limit of the pH of the buffer is not particularly limited, it is preferably 4.5 or higher, 5.5 or higher, or 6.0 or higher from the viewpoint of irritation to the skin or body hair.
- the second agent of the present disclosure contains a chelating agent and can swell the hyaluronic acid described above. Being able to swell hyaluronic acid means, in other words, that the chelating agent is contained in the second agent in an amount that allows the hyaluronic acid to swell, as shown in FIG. 1 or FIG. is intended. If the chelating agent is contained in the second agent at a rate that allows the hyaluronic acid to swell, it can be said that the cations that neutralize the carboxyl groups in the hyaluronic acid can be sufficiently captured by the chelating agent. .
- the carboxyl group in hyaluronic acid with dissociated cations can sufficiently express the ability to hold water (hydration capacity), and swollen hyaluronic acid retains more water than compacted hyaluronic acid.
- Such hyaluronic acid can provide good moisturizing properties to the skin due to its increased hydrostatic capacity.
- Swelling of hyaluronic acid means that the volume of hyaluronic acid in the first agent increases when the second agent is applied to the first agent.
- the increase in the volume of hyaluronic acid It can be evaluated by a ratio based on particle size (sometimes referred to as “particle size ratio”) or a ratio based on partial specific volume (sometimes referred to as “partial specific volume ratio").
- the particle size ratio can be greater than 1.00, 1.10 or more, 1.20 or more, or 1.30 or more. Although the upper limit of the particle size ratio is not particularly limited, it can be, for example, 3.00 or less, 2.50 or less, 2.00 or less, or 1.80 or less.
- the partial specific volume ratio can be greater than 1.00, 1.01 or more, or 1.02 or more. Although the upper limit of the partial specific volume ratio is not particularly limited, it can be, for example, 1.20 or less, 1.15 or less, or 1.10 or less.
- "partial specific volume” means the amount of change in the total volume (cm 3 /g) when 1 g of hyaluronic acid is dissolved in an infinite solvent while keeping the temperature, pressure and concentrations of all other components constant.
- V 0 sp,hya is the partial specific volume of hyaluronic acid
- ⁇ is the density of the hyaluronic acid aqueous solution
- w hya is the weight fraction of hyaluronic acid.
- Partial specific volume ratio Partial specific volume of hyaluronic acid in the state where a predetermined amount of chelating agent is blended in the first agent / Partial specific volume of hyaluronic acid in the first agent that does not contain a chelating agent ...
- the chelating agent that can be blended in the second agent of the present disclosure is particularly limited as long as it is a chelating agent that can swell hyaluronic acid by trapping cations that electrostatically shield the negative charge of the carboxyl group of hyaluronic acid. no.
- chelating agents include ethylenediaminetetraacetic acid, disodium ethylenediaminetetraacetic acid, trisodium ethylenediaminetetraacetic acid, nitrilotriacetic acid, sodium nitrilotriacetate, ammonium nitrilotriacetic acid, hydroxyethylethylenediaminetriacetic acid, and hydroxyethylethylenediaminetriacetic acid.
- a chelating agent can be used individually or in combination of 2 or more types. Among them, disodium ethylenediaminetetraacetate (EDTA), hydroxyethyliminodiacetic acid (HIDA), and diethylenetriaminepentaacetic acid (DTPA) are used from the viewpoint of the cation trapping property and the moisturizing effect of hyaluronic acid accompanying this cation trapping. , nitrilotriacetic acid, phytic acid and sodium hexametaphosphate (HMP) are preferred.
- EDTA disodium ethylenediaminetetraacetate
- HIDA hydroxyethyliminodiacetic acid
- DTPA diethylenetriaminepentaacetic acid
- HMP sodium hexametaphosphate
- the amount of the chelating agent in the second agent is such that the particle size ratio or the partial specific volume ratio of hyaluronic acid increases depending on the type and amount of hyaluronic acid or salt in the first agent and the type of chelating agent. It can be appropriately set within the range.
- the amount of the chelating agent per 100 mol of the salt is 0.001 or more, 0 0.01 or more, 0.05 or more, 0.07 or more, 0.10 or more, 0.15 or more, 0.20 or more, 0.25 or more, or 0.30 or more, and 10 or less, It can be 7.0 or less, 5.0 or less, 3.0 or less, 2.0 or less, 1.7 or less, or 1.5 or less.
- the amount of the chelating agent per 100 mol of salt is 0.1 or more, 0.5 1.0 or more, 1.2 or more, 1.5 or more, 1.7 or more, or 2.0 or more; .0 or less, 4.5 or less, or 4.0 or less.
- a second agent of the present disclosure may typically comprise an aqueous medium.
- the aqueous medium is not particularly limited, and any aqueous medium used for cosmetics, quasi-drugs, etc. can be used.
- ion-exchanged water, distilled water, ultrapure water, tap water can be used.
- An aqueous medium can be used individually or in combination of 2 or more types.
- the first agent and second agent of the cosmetic composition of the present disclosure can appropriately contain various components within a range that does not affect the effects of the present invention.
- Such ingredients include, for example, skin or hair nutrients, vitamins, pharmaceuticals, quasi-drugs, water-soluble agents applicable to cosmetics, ultraviolet absorbers, antioxidants, preservatives, antioxidant aids, Thickeners, pigments, dyes, dyes, perfumes and the like can be mentioned.
- Optional components can be used alone or in combination of two or more.
- the first agent and second agent of the cosmetic of the present disclosure can be prepared, for example, using the following method.
- various materials such as hyaluronic acid, salts, chelating agents, water, buffers, and optional ingredients that can be used in the method for preparing the first agent and the second agent can be the various materials described above.
- the first agent can be prepared by adding a salt to water or a buffer to prepare a solution, adding hyaluronic acid to this solution, and dissolving the hyaluronic acid while stirring and mixing.
- hyaluronic acid can be blended with water or a buffer solution, stirred and mixed to dissolve hyaluronic acid, and then a salt can be further blended to prepare the first agent.
- the buffer solution itself exhibits the above-described salt concentration or ionic strength due to the action of the salt contained in the buffer solution, the addition of salt can be omitted.
- optional ingredients When the above-mentioned optional ingredients are blended, such optional ingredients may be blended before compacting hyaluronic acid with a salt. It is preferably added after the acid is prepared.
- a second agent can be prepared by blending a chelating agent with water and stirring and mixing.
- the cosmetic of the present disclosure can be applied to any part of the body, for example, to any part on the surface of the skin (body surface) or body hair (hair).
- body surface skin
- hair hair
- the skin of the face lips, eyes, eyelids, cheeks, forehead, eyebrows, nose, etc.
- head head
- ears ears
- hands arms, neck, legs, feet
- chest abdomen, back, etc.
- body hair also intends hair growing on the body.
- Body hair also be referred to as "hair” in the present disclosure.
- the cosmetics of the present disclosure can be suitably used as skin cosmetics or hair cosmetics.
- a cosmetic method using the cosmetic of the present disclosure includes applying the first agent described above to the body surface or body hair, and then applying the second agent described above to the surface to which the first agent is applied.
- the term “beauty method” refers to a method of beautifying a body surface or body hair by applying the cosmetic composition of the present disclosure to the body surface or body hair. Or it is different from the method of diagnosis.
- the cosmetic of the present disclosure allows the compacted hyaluronic acid to remain in the skin grooves or pores, or adsorb to the surface of body hair, and in some cases, penetrates into the skin or body hair. Then, cations such as sodium ions that neutralize the negative charge of the carboxyl group in hyaluronic acid are captured and swollen, and the moisturizing property of hyaluronic acid itself is fully expressed to improve skin or body hair. It can moisturize well. As a result, for example, the function of generating moisturizing ingredients produced by the skin itself is improved, and the malfunction of turnover in the stratum corneum is improved, or the moisture of the hair is improved, resulting in rough skin or split ends. Alternatively, troubles such as hair breakage are less likely to occur, and the cosmetic effect can be enhanced.
- the means for applying the first and second agents to the body surface or body hair is not particularly limited, and for example, the first and second agents can be applied to the body surface or body hair.
- each spray container containing the first agent or the second agent may be used to spray the skin or body hair.
- the first agent or second agent is put into a container that does not have a spray function, and an appropriate amount of the first agent or second agent is collected from such a container on a finger or palm and applied to the body surface or body hair. It may be carried out by spreading each.
- the second agent containing a chelating agent when using the second agent containing a chelating agent, after applying the first agent to the skin in the above amount, the second agent was further applied to the skin in the above amount to the applied part.
- the water content values in Table 4 show the average value of six times, and the "difference" is the value obtained by subtracting the measured value before coating from each measured value.
- the second agent containing a chelating agent when using the second agent containing a chelating agent, after applying the first agent to the skin in the above amount, the second agent was further applied to the skin in the above amount to the applied part.
- the value of the number of textures in Table 5 indicates the average value of 6 times.
- Test Example 1 Effect of chelating agent>
- HMP substance amount converted into metaphosphoric acid
- Hyaluronic acid manufactured by Shiseido Co., Ltd., Biohyalo 12: weight average molecular weight 1,200,000
- Hyaluronic acid manufactured by Shiseido Co., Ltd., Biohyalo 12: weight average molecular weight 1,200,000
- magnesium chloride hexahydrate (MgCl 2 .6H 2 O) for each fractionated composition A %, or sodium chloride was added at concentrations of 0.82% by mass and 1.23% by mass, and stirred and mixed with a vortex mixer to prepare test samples containing no chelating agent.
- HMP sodium hexametaphosphate
- Test Example 2 Type of chelating agent>
- HMP sodium hexametaphosphate
- Table 3 shows the results.
- the “control” in Table 3 is a test sample containing salt and hyaluronic acid, which does not contain a chelating agent, and serves as a reference for comparison of particle size ratios.
- EDTA disodium ethylenediaminetetraacetate
- HIDA hydroxyethyliminodiacetic acid
- DTPA means diethylenetriaminepentaacetic acid.
- test sample was prepared in the same manner as in Test Example 1 using each chelating agent listed in Table 3.
- magnesium chloride hexahydrate MgCl 2 .6H 2 O
- concentration of the chelating agent was set to 0.03% by mass.
- Test Example 3 Evaluation of moisturizing property (keratin moisture content)>
- evaluation of moisturizing properties was examined based on changes in the water content of the stratum corneum with time for each test sample. The results are shown in Table 4 and FIG.
- Hyaluronic acid manufactured by Shiseido Co., Ltd., Biohyalo 12: weight average molecular weight 1,200,000
- Hyaluronic acid manufactured by Shiseido Co., Ltd., Biohyalo 12: weight average molecular weight 1,200,000
- a composition Magnesium chloride hexahydrate (MgCl 2 .6H 2 O) was added to this composition at a concentration of 1.42% by mass, and the mixture was stirred and mixed with a vortex mixer to prepare a test sample of the first agent.
- HMP sodium hexametaphosphate
- Comparative example 1 The first agent of Example 1 was used as a test sample of Comparative Example 1.
- Comparative example 2 The second agent of Example 1 was used as a test sample of Comparative Example 2.
- Test Example 4 Evaluation of moisturizing property (skin texture number)>
- the evaluation of the moisturizing property was examined based on the time-dependent changes in the number of skin textures of each test sample. The results are shown in Table 5 and FIG.
- Example 2 The first and second agents of Example 1 were used as test samples of Example 2.
- Comparative Example 3 The first agent of Example 1 was used as a test sample of Comparative Example 3.
- Comparative Example 4 The second agent of Example 1 was used as a test sample of Comparative Example 4.
- the average particle size of the hyaluronic acid particles in the composition was measured using a Zetasizer (manufactured by Malvern Panalytical) or a dynamic light scattering photometer DLS-8000 (manufactured by Otsuka Electronics Co., Ltd.), and Z by a dynamic light scattering method. Evaluation was based on the average particle size.
- Hyaluronic acid manufactured by Shiseido Co., Ltd., Biohyalo 12: weight average molecular weight 1,200,000
- Hyaluronic acid manufactured by Shiseido Co., Ltd., Biohyalo 12: weight average molecular weight 1,200,000
- sodium chloride was added at concentrations of 0.01 M (mol/l), 0.003 M, 0.01 M, 0.02 M, 0.03 M, and 0.10 M, and stirred and mixed with a vortex mixer to obtain hyaluron.
- Each acid particle-containing composition was prepared.
- the concentration of sodium chloride coincides with the ionic strength.
- composition (Method for preparing composition)
- concentration of hyaluronic acid when preparing the composition was 0.01% by mass, 0.1% by mass, 0.2% by mass, 0.3% by mass, 0.4% by mass, and 0.5% by mass, and the ionic strength was
- Each composition containing hyaluronic acid particles was prepared in the same manner as in Reference Test Example 1, except that sodium chloride was blended in the proportions shown in Table 7.
- Hyaluronic acid was prepared in the same manner as in Reference Test Example 1, except that the concentration of hyaluronic acid was set to 0.4% by mass and 0.5% by mass, and sodium chloride was added so that the ionic strength was the ratio described in Table 8. Each acid particle-containing composition was prepared.
- ⁇ Reference Test Example 4 Effect of particle size of hyaluronic acid particles on moisture retention>
- Reference Test Example 4 the influence of the particle size of the hyaluronic acid particles on the moisturizing properties was examined. The results are shown in Table 9 and FIG. Here, it can be said that, as the water content ratio is greater than 1, the moisturizing performance is improved compared to the state before application of the composition.
- the water content ratio is preferably 1.25 or more, more preferably 1.30 or more, and particularly preferably 1.35 or more.
- composition containing hyaluronic acid particles was prepared in the same manner as in Reference Test Example 1, except that the concentration of hyaluronic acid was 0.4% by mass, and sodium chloride was added so that the ionic strength was the proportion shown in Table 9. each prepared.
- the hyaluronic acid molecules in the composition with an ionic strength of 0 to which sodium chloride is not added are considered to spread like threads and not take the form of particles. It is written.
- Hyaluronic acid manufactured by Shiseido Co., Ltd., Biohyalo 12: weight average molecular weight 1,200,000
- citric acid buffer manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.: pH 6.5, ionic strength 0.006 0.1% by mass It added so that it might become content, and it stirred and mixed with the vortex mixer, and the composition C was prepared.
- sodium citrate was added to each of the fractionated compositions C so that the ionic strength of the salt was 0.03, 0.06, and 0.30, and the mixture was mixed with a vortex mixer. to prepare each composition containing hyaluronic acid particles.
- the concentration of sodium citrate when the ionic strength is 0.03 is 0.005 M
- the concentration of sodium citrate when the ionic strength is 0.06 is 0.010 M
- the ionic strength is The concentration of sodium citrate at 0.30 was 0.050M.
- Hyaluronic acid manufactured by Shiseido Co., Ltd., Biohyalo 12: weight average molecular weight 1,200,000
- Hyaluronic acid was added to deionized water so that the content was 0.1% by mass, and the mixture was stirred and mixed with a vortex mixer to prepare composition D.
- sodium chloride is added at a concentration of 0.10 M to composition D so that the ionic strength of the salt is 0.10, and mixed by stirring with a vortex mixer to contain hyaluronic acid particles.
- a composition was prepared.
- Hyaluronic acid manufactured by Shiseido Co., Ltd., Biohyalo 12: weight average molecular weight 1,200,000
- isotonic phosphate buffer manufactured by Takara Bio Co., Ltd.: pH 7.4, ionic strength 0.154
- Reference Comparative Example 1 A composition of Reference Comparative Example 1 was prepared by blending 10% by mass of urea with respect to the total amount of the hyaluronic acid particle-containing composition of Reference Example 1.
- Reference Comparative Example 2 A composition of Reference Comparative Example 2 was prepared by blending 10% by mass of urea with respect to the total amount of the hyaluronic acid particle-containing composition of Reference Example 2.
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Abstract
Description
無機塩及び有機酸塩からなる群から選択される少なくとも一種の塩、並びにヒアルロン酸を含む第1剤、並びに、
キレート剤を含む、前記ヒアルロン酸を膨潤させるための第2剤、を含む、
化粧料。
〈態様2〉
前記第1剤中のヒアルロン酸の体積が、前記第1剤に対して前記第2剤を適用すると増大する、態様1に記載の化粧料。
〈態様3〉
前記ヒアルロン酸が、前記第1剤の全量に対し、0.005質量%以上含まれている、態様1又は2に記載の化粧料。
〈態様4〉
前記塩を構成する陽イオンが、金属イオンである、態様1~3のいずれかに記載の化粧料。
〈態様5〉
前記キレート剤が、エチレンジアミン四酢酸、エチレンジアミン四酢酸二ナトリウム、エチレンジアミン四酢酸三ナトリウム、ニトリロ三酢酸、ニトリロ三酢酸ナトリウム、ニトリロ三酢酸アンモニウム、ヒドロキシエチルエチレンジアミン三酢酸、ヒドロキシエチルエチレンジアミン三酢酸ナトリウム、ペンテト酸、ペンテト酸五ナトリウム、トリエチレンテトラミン六酢酸、トリエチレンテトラミン六酢酸ナトリウム、イミジコハク酸、イミジコハク酸四ナトリウム、エチレンジアミン二コハク酸、エチレンジアミン二コハク酸三ナトリウム、ヒドロキシエチルイミノ二酢酸、ヒドロキシエチルイミノ二酢酸二ナトリウム、イミノ二コハク酸、イミノ二コハク酸四ナトリウム、トリエチレンテトラミン六酢酸、トリエチレンテトラミン六酢酸ナトリウム、メチルグリシン二酢酸、メチルグリシン二酢酸三ナトリウム、ヒドロキシイミノジコハク酸、ヒドロキシイミノジコハク酸四ナトリウム、L-アスパラギン酸二酢酸L-アスパラギン酸二酢酸四ナトリウム、グルタミン酸ジ酢酸、グルタミン酸ジ酢酸四ナトリウム、プロパンジアミン四酢酸、エチレンジアミン四酢酸二アンモニウム、1,3-ジアミノ-2-ヒドロキシプロパン-四酢酸、1,3-ジアミノ-2-ヒドロキシプロパン-四酢酸、N,N-ビス(2-ヒドロキシエチル)グリシン、グリコールエーテルジアミン四酢酸、二カルボキシメチルグルタミン酸、二カルボキシメチルグルタミン酸四ナトリウム、ジエチレントリアミン五酢酸、ヘキサメタリン酸、ヘキサメタリン酸ナトリウム、ニトリロトリス(メチレンホスホン酸)、ニトリロトリス(メチレンホスホン酸)カリウム、2-ホスホノブタン-1,2,4-トリカルボン酸、エチレンジアミンテトラメチレンホスホン酸、エチレンジアミンテトラメチレンホスホン酸五ナトリウム、フィチン酸、及びクエン酸からなる群から選択される少なくとも一種である、態様1~4のいずれかに記載の化粧料。
〈態様6〉
前記ヒアルロン酸の重量平均分子量が、10,000,000以下である、態様1~5のいずれかに記載の化粧料。
〈態様7〉
態様1~6のいずれかに記載の化粧料を使用する美容方法であって、
前記第1剤を体表又は体毛に適用した後に、当該第1剤の適用面に対して前記第2剤を適用する、
美容方法。
本開示の化粧料は第1剤及び第2剤を含む。
本開示の第1剤は、無機塩及び有機酸塩からなる群から選択される少なくとも一種の塩、並びにヒアルロン酸を含んでいる。
本開示の第1剤に配合し得る塩としては、ヒアルロン酸のマイナス電荷を見掛け上中和できる塩であれば特に制限はない。このような塩として、無機塩及び有機酸塩から選択される少なくとも一種の塩を挙げることができる。化粧料としての使用を考慮した場合、無機塩及び有機酸塩の中でも、皮膚又は体毛に対して悪影響を及ぼしにくい塩であることが好ましい。ここで、「無機塩」とは、無機成分のみから構成される塩を意味し、無機酸と無機塩基より生じるイオンから構成される塩と言い換えることもできる。また、「有機酸塩」とは、有機酸と金属イオンが結合してできた塩を意味する。なお、塩は、第1剤中では、一般に、塩由来のイオンの形態で存在している。したがって、本開示において、例えば「塩を含む第1剤」とは、このようなイオンの形態で塩が含まれていることを意図する。また、イオン性界面活性剤は、本開示の「塩」には包含されない。
本開示の第1剤に配合し得るヒアルロン酸としては特に制限はない。一般には、ヒアルロン酸は、N-アセチル-D-グルコサミン残基と、D-グルクロン酸残基が交互に結合した直鎖状高分子を意味し、かかるヒアルロン酸は、例えば、鶏冠若しくは他の動物組織からの単離抽出、又はストレプト・コッカス属などの微生物を用いた発酵法により得ることができる。
本開示の第1剤は、典型的には水性媒体を含み得る。かかる水性媒体としては特に制限はなく、化粧料、医薬部外品等に使用される水性媒体を使用することができる。例えば、イオン交換水、蒸留水、超純水、水道水、緩衝液等を使用することができる。水性媒体は単独で又は二種以上組み合わせて使用することができる。
本開示の第2剤は、キレート剤を含んでおり、上述したヒアルロン酸を膨潤させることができる。ヒアルロン酸を膨潤させることができるということは、言い換えると、図1又は図2に示されるような、ヒアルロン酸を膨潤させ得るような範囲の量で、キレート剤が第2剤中に含まれることを意図している。ヒアルロン酸を膨潤させ得る割合で、キレート剤が第2剤中に含まれていれば、ヒアルロン酸中のカルボキシル基を中和させている陽イオンをキレート剤で十分に捕捉することができるといえる。陽イオンが乖離したヒアルロン酸中のカルボキシル基は、水を抱え込む性能(水和能)を十分に発現することができるようになり、また、膨潤したヒアルロン酸はコンパクト化したヒアルロン酸に比べて保水力が増加するため、このようなヒアルロン酸は肌に対して良好な保湿性を提供することができる。
粒子径比=キレート剤を所定量配合した第1剤中のヒアルロン酸粒子の平均粒子径/キレート剤を含まない第1剤中のヒアルロン酸粒子の平均粒子径 …式1
V0 sp,hyaは、ヒアルロン酸の部分比容であり、
ρは、ヒアルロン酸水溶液の密度であり、
whyaは、ヒアルロン酸の重量分率である。)
本開示の第2剤に配合し得るキレート剤としては、ヒアルロン酸のカルボキシル基のマイナス電荷を静電遮蔽している陽イオンを捕捉し、ヒアルロン酸を膨潤化させ得るキレート剤であれば特に制限はない。このようなキレート剤として、例えば、エチレンジアミン四酢酸、エチレンジアミン四酢酸二ナトリウム、エチレンジアミン四酢酸三ナトリウム、ニトリロ三酢酸、ニトリロ三酢酸ナトリウム、ニトリロ三酢酸アンモニウム、ヒドロキシエチルエチレンジアミン三酢酸、ヒドロキシエチルエチレンジアミン三酢酸ナトリウム、ペンテト酸、ペンテト酸五ナトリウム、トリエチレンテトラミン六酢酸、トリエチレンテトラミン六酢酸ナトリウム、イミジコハク酸、イミジコハク酸四ナトリウム、エチレンジアミン二コハク酸、エチレンジアミン二コハク酸三ナトリウム、ヒドロキシエチルイミノ二酢酸、ヒドロキシエチルイミノ二酢酸二ナトリウム、イミノ二コハク酸、イミノ二コハク酸四ナトリウム、トリエチレンテトラミン六酢酸、トリエチレンテトラミン六酢酸ナトリウム、メチルグリシン二酢酸、メチルグリシン二酢酸三ナトリウム、ヒドロキシイミノジコハク酸、ヒドロキシイミノジコハク酸四ナトリウム、L-アスパラギン酸二酢酸L-アスパラギン酸二酢酸四ナトリウム、グルタミン酸ジ酢酸、グルタミン酸ジ酢酸四ナトリウム、プロパンジアミン四酢酸、エチレンジアミン四酢酸二アンモニウム、1,3-ジアミノ-2-ヒドロキシプロパン-四酢酸、1,3-ジアミノ-2-ヒドロキシプロパン-四酢酸、N,N-ビス(2-ヒドロキシエチル)グリシン、グリコールエーテルジアミン四酢酸、二カルボキシメチルグルタミン酸、二カルボキシメチルグルタミン酸四ナトリウム、ジエチレントリアミン五酢酸、ヘキサメタリン酸、ヘキサメタリン酸ナトリウム、ニトリロトリス(メチレンホスホン酸)、ニトリロトリス(メチレンホスホン酸)カリウム、2-ホスホノブタン-1,2,4-トリカルボン酸、エチレンジアミンテトラメチレンホスホン酸、エチレンジアミンテトラメチレンホスホン酸五ナトリウム、フィチン酸、及びクエン酸を挙げることができる。キレート剤は、単独で又は二種以上組み合わせて使用することができる。なかでも、陽イオンの捕捉性、及びこの陽イオンの捕捉に伴うヒアルロン酸の保湿効果の観点から、エチレンジアミン四酢酸二ナトリウム(EDTA)、ヒドロキシエチルイミノ二酢酸(HIDA)、ジエチレントリアミン五酢酸(DTPA)、ニトリロ三酢酸、フィチン酸、及びヘキサメタリン酸ナトリウム(HMP)が好ましい。
本開示の第2剤は、典型的には水性媒体を含み得る。水性媒体としては特に制限はなく、化粧料、医薬部外品等に使用される水性媒体を使用することができる。例えば、イオン交換水、蒸留水、超純水、水道水を使用することができる。水性媒体は単独で又は二種以上組み合わせて使用することができる。
本開示の化粧料の第1剤及び第2剤は、本発明の効果に影響を及ぼさない範囲で、各種成分を適宜配合することができる。このような成分としては、例えば、皮膚又は毛髪栄養剤、ビタミン、医薬品、医薬部外品、化粧品等に適用可能な水溶性薬剤、紫外線吸収剤、酸化防止剤、防腐剤、酸化防止助剤、増粘剤、顔料、染料、色素、香料等を挙げることができる。任意成分は、単独で又は二種以上組み合わせて使用することができる。
本開示の化粧料の第1剤及び第2剤は、例えば以下の方法を用いて調製することができる。なお、第1剤及び第2剤の調製方法で使用し得る、ヒアルロン酸、塩、キレート剤、水、緩衝液、任意成分等の各種材料については、上述した各種材料を使用することができる。
水又は緩衝液に塩を配合して溶液を調製し、この溶液にヒアルロン酸を配合し、攪拌混合しながらヒアルロン酸を溶解させて第1剤を調製することができる。
水にキレート剤を配合し、攪拌混合して第2剤を調製することができる。
本開示の化粧料は、体のあらゆる部分に適用することができ、例えば、皮膚の表面(体表)上又は体毛(毛髪)上のいかなる箇所に適用することができる。具体的には、例えば、顔(唇、目元、瞼、頬、額、眉間、鼻など)、頭(頭皮)、耳、手、腕、首、脚、足、胸、腹、背中等の皮膚表面、又は髪の毛、まつ毛、眉毛、髭等の体毛に対して適宜適用することができる。ここで、皮膚には、皮膚の表皮の角質が変化して硬化した爪なども含まれる。また、体毛は、体に生えている毛を意図する。本開示において「体毛」は「毛髪」と称することもできる。
本開示の化粧料を用いた美容方法は、上述した第1剤を体表又は体毛に適用した後に、この第1剤の適用面に対して上述した第2剤を適用することを含む。なお、本開示において「美容方法」とは、本開示の化粧料を体表又は体毛に対して適用して体表又は体毛の状態を美しく整えて美化する方法を意味し、人間を手術、治療又は診断する方法とは相違する。
〈皮膚化粧料の評価〉
下記の製造方法により得た各試験サンプルを用いて以下に示す各種評価を実施し、その結果を、表1~5及び図1~4にまとめる。
試験サンプル中のヒアルロン酸粒子の平均粒子径について、ゼータサイザー(マルバーン・パナリティカル社製)を用い、動的光散乱法によるZ平均粒子径に基づいて評価した。得られた各平均粒子径と下記式4から粒子径比を算出した:
粒子径比=キレート剤を所定量配合した試験サンプル中のヒアルロン酸粒子の平均粒子径/キレート剤を含まない試験サンプル中のヒアルロン酸粒子の平均粒子径 …式4
被験者の上腕内側部を石鹸(サボンドール(商標))にて洗浄後、温度25±1℃、相対湿度50±5%の恒温恒湿室にて15分間過ごしてもらい、被験者の環境調整を行った。次いで、洗浄した上腕内側部の皮膚表面における試験サンプル適用前の水分量、並びに試験サンプルを皮膚表面に対して2μl/cm2の割合で18μl塗布してから30分後及び90分後の水分量を、コルネオメーター(商標)CM825(Courage and Khazaka社製)を用いて測定した。ここで、キレート剤を含む第2剤を使用する場合には、第1剤を上記の量で皮膚に塗布した後、その塗布部に対して第2剤をさらに上記の量で皮膚に塗布した。また、表4中の水分量の値は、6回の平均値を示しており、「差分」とは、各実測値から塗布前の実測値を差し引いた値である。
被験者の上腕内側部を石鹸(サボンドール(商標))にて洗浄後、温度25±1℃、相対湿度50±5%の恒温恒湿室にて15分間過ごしてもらい、被験者の環境調整を行った。次いで、洗浄した上腕内側部の皮膚表面における試験サンプル適用前のきめ数、並びに試験サンプルを皮膚表面に対して2μl/cm2の割合で18μl塗布してから30分後及び90分後、のきめ数を、ハンディスキンセンサーII(株式会社資生堂製)を用いて測定した。ここで、キレート剤を含む第2剤を使用する場合には、第1剤を上記の量で皮膚に塗布した後、その塗布部に対して第2剤をさらに上記の量で皮膚に塗布した。また、表5中のきめ数の値は、6回の平均値を示している。
試験例1では、塩を配合してコンパクト化したヒアルロン酸に及ぼすキレート剤の影響について検討した。その結果を表1~2及び図1~2に示す。ここで、キレート剤(HMP)の物質量は、メタリン酸(P2O5)に換算した物質量である。
ヒアルロン酸(株式会社資生堂製、バイオヒアロ12:重量平均分子量120万)をイオン交換水中に0.5質量%の含有量となるように添加し、ボルテックスミキサーで攪拌混合して組成物Aを調製した。ヒアルロン酸を溶解させた後、分取した各組成物Aに対し、塩化マグネシウム六水和物(MgCl2・6H2O)を0.46質量%、0.91質量%、及び1.42質量%の濃度で添加し、又は塩化ナトリウムを0.82質量%、及び1.23質量%の濃度で添加し、ボルテックスミキサーで攪拌混合してキレート剤を含まない試験サンプルを各々調製した。
表1~2及び図1~2の結果から明らかなように、塩を添加してコンパクト化したヒアルロン酸に対し、キレート剤を所定の割合で配合すると、ヒアルロン酸の粒子径比が大きくなる、すなわち、ヒアルロン酸が膨潤することが確認できた。このヒアルロン酸の膨潤は、キレート剤が、ヒアルロン酸のカルボキシル基のマイナス電荷を静電遮蔽している陽イオンを捕捉したためであると考えられる。
試験例2では、ヘキサメタリン酸ナトリウム(HMP)以外の他のキレート剤による、塩を配合してコンパクト化したヒアルロン酸の膨潤性について検討した。その結果を表3に示す。ここで、表3中の「コントロール」とは、キレート剤を含まない、塩とヒアルロン酸を含む試験サンプルであって、粒子径比の比較の基準となる試験サンプルである。また、表3中の「EDTA」は、エチレンジアミン四酢酸二ナトリウムを意味し、「HIDA」は、ヒドロキシエチルイミノ二酢酸を意味し、「DTPA」は、ジエチレントリアミン五酢酸を意味する。
表3に記載される各キレート剤を用いて、試験例1と同様の方法で試験サンプルを調製した。ここで、塩としては、塩化マグネシウム六水和物(MgCl2・6H2O)を使用し、塩濃度は1.42質量%とした。また、キレート剤の濃度は、いずれも0.03質量%とした。
表3の結果から明らかなように、ヘキサメタリン酸ナトリウム(HMP)以外の他のキレート剤を用いた場合でも、ヒアルロン酸が膨潤することが確認できた。
試験例3では、各試験サンプルによる角層水分量の経時変化から、保湿性についての評価を検討した。その結果を表4及び図3に示す。
ヒアルロン酸(株式会社資生堂製、バイオヒアロ12:重量平均分子量120万)をイオン交換水中に0.5質量%の含有量となるように添加し、ボルテックスミキサーで攪拌混合して組成物を調製した。この組成物に対し、塩化マグネシウム六水和物(MgCl2・6H2O)を1.42質量%の濃度で添加し、ボルテックスミキサーで攪拌混合して第1剤の試験サンプルを調製した。
実施例1の第1剤を、比較例1の試験サンプルとして使用した。
実施例1の第2剤を、比較例2の試験サンプルとして使用した。
表4及び図3の結果から明らかなように、塩を添加してコンパクト化したヒアルロン酸を肌に塗布した後に、キレート剤を適用すると、角質水分量が大幅に上昇することが確認できた。これは、ヒアルロン酸中のカルボキシル基のマイナス電荷を中和させていたマグネシウムイオンが、キレート剤によって捕捉された結果、ヒアルロン酸自体が有する保湿性能が十分に発現するとともに、ヒアルロン酸が膨潤して保水力が増加したためであると考えられる。キレート剤による陽イオンの捕捉に関する結果は、上述した表1~2及び図1~2の結果とも整合している。
試験例4では、各試験サンプルによる肌のきめ数の経時変化から、保湿性についての評価を検討した。その結果を表5及び図4に示す。
実施例1の第1剤及び第2剤を、実施例2の試験サンプルとして使用した。
実施例1の第1剤を、比較例3の試験サンプルとして使用した。
実施例1の第2剤を、比較例4の試験サンプルとして使用した。
表5及び図4の結果から明らかなように、塩を添加してコンパクト化したヒアルロン酸を肌に塗布した後に、キレート剤を適用すると、肌のきめ数が上昇することが確認できた。これは、上述した表4及び図3の結果で示されたように、実施例1の第1剤及び第2剤を肌に適用することで角質水分量が増加し、肌のきめがふっくらと整ったためであると考えられる。
参考のため、ヒアルロン酸が塩によって粒子のようにコンパクト化し得ること、及びこのようなヒアルロン酸粒子が及ぼす作用について以下に説明する。
下記の製造方法により得た組成物に対し、以下に示す各種評価を実施し、その結果を、表6~11及び図5~10にまとめる。なお、表及び図面中の「HA」は、ヒアルロン酸を意図する。
組成物中のヒアルロン酸粒子の平均粒子径については、ゼータサイザー(マルバーン・パナリティカル社製)、又はダイナミック光散乱光度計DLS-8000(大塚電子社製)を用い、動的光散乱法によるZ平均粒子径に基づいて評価した。
被験者の上腕内側部を石鹸にて洗浄後、温度21±1℃、相対湿度45±5%の恒温恒湿室にて20分間過ごしてもらい、被験者の環境調整を行った。次いで、洗浄した上腕内側部の皮膚表面における組成物適用前の水分量、並びに組成物を皮膚表面に対して1滴(2×2cm2)塗布してから20分後、30分後、60分後及び120分後の水分量を、コルネオメーター(商標)CM825(Courage and Khazaka社製)を用いて測定した。得られた各水分量から以下の式5によって水分量比を算出した:
水分量比=組成物適用後の水分量/組成物適用前の水分量 …式5
参考試験例1では、ヒアルロン酸粒子の粒子径に及ぼすイオン強度の影響について検討した。その結果を表6及び図5に示す。
ヒアルロン酸(株式会社資生堂製、バイオヒアロ12:重量平均分子量120万)をイオン交換水中に0.1質量%の含有量となるように添加し、ボルテックスミキサーで攪拌混合して組成物Bを調製した。ヒアルロン酸を溶解させた後、塩のイオン強度が、0.001、0.003、0.01、0.02、0.03、及び0.10となるように、分取した各組成物Bに対し、塩化ナトリウムを、0.01M(mol/l)、0.003M、0.01M、0.02M、0.03M、及び0.10Mの濃度で添加し、ボルテックスミキサーで攪拌混合してヒアルロン酸粒子含有組成物を各々調製した。ここで、1価の陽イオンと1価のマイナス電荷から構成される塩化ナトリウムの場合には、塩化ナトリウムの濃度とイオン強度の値は一致する。
表6及び図5の結果から明らかなように、塩を添加することによってナノメーターオーダーのヒアルロン酸粒子が得られることが確認できた。また、塩の添加量の増加、即ち、イオン強度の増加に伴い、ヒアルロン酸粒子の粒子径は減少する傾向を示し、特に、イオン強度が0.03以上において、100nm以下のヒアルロン酸粒子が得られることが確認できた。
参考試験例2では、ヒアルロン酸粒子の粒子径に及ぼす組成物調製時のヒアルロン酸の濃度とイオン強度の影響について検討した。その結果を表7及び図6に示す。
組成物調製時のヒアルロン酸の濃度を0.01質量%、0.1質量%、0.2質量%、0.3質量%、0.4質量%、0.5質量%とし、イオン強度が表7に記載される割合となるように塩化ナトリウムを配合したこと以外は、参考試験例1と同様にしてヒアルロン酸粒子含有組成物を各々調製した。
表7及び図6の結果から明らかなように、ヒアルロン酸の濃度が上がっても、塩を添加することによってナノメーターオーダーのヒアルロン酸粒子が得られることが確認できた。
参考試験例3では、組成物調製時のヒアルロン酸の濃度が0.4~0.5質量%のときの、ヒアルロン酸粒子に及ぼすイオン強度の影響について検討した。その結果を表8及び図7に示す。
ヒアルロン酸の濃度を0.4質量%、0.5質量%とし、イオン強度が表8に記載される割合となるように塩化ナトリウムを配合したこと以外は、参考試験例1と同様にしてヒアルロン酸粒子含有組成物を各々調製した。
表8及び図7の結果から明らかなように、ヒアルロン酸の濃度が0.4質量%及び0.5質量%のいずれの場合も、イオン強度が0.05以上であれば、200nm以下のヒアルロン酸粒子が得られることが確認できた。特に、ヒアルロン酸の濃度が0.4質量%の場合には、イオン強度が0.20~1.0の範囲において、100nm以下のヒアルロン酸粒子が得られることが確認できた。
参考試験例4では、保湿性に及ぼすヒアルロン酸粒子の粒子径の影響について検討した。その結果を表9及び図8に示す。ここで、水分量比は、1よりも大きくなればなるほど、組成物適用前の状態に比べて保湿性能が向上しているといえる。水分量比は、1.25以上であることが好ましく、1.30以上であることがより好ましく、1.35以上であることが特に好ましい。
ヒアルロン酸の濃度を0.4質量%とし、イオン強度が表9に記載される割合となるように塩化ナトリウムを配合したこと以外は、参考試験例1と同様にしてヒアルロン酸粒子含有組成物を各々調製した。ここで、塩化ナトリウムを添加していないイオン強度0の組成物中のヒアルロン酸分子は、糸状に広がり、粒子の形態をとっていないと考えられるため、表及び図中には「非粒子」と表記している。
表9及び図8の結果から明らかなように、粒子化していないヒアルロン酸を含む組成物、及び平均粒子径が294nm以上のヒアルロン酸粒子を含有する組成物の場合には、組成物を皮膚に適用した直後は、保湿性能が一時的に上昇しているが、その保湿性能はわずか30分程度で低下しており、組成物を適用していない状態とほぼ同程度の保湿性能しか示さなかった。これは、これらの組成物中のヒアルロン酸が皮膚内部まで侵入していないためであると考えられる。
参考試験例5では、クエン酸ナトリウムによるヒアルロン酸粒子の粒子径の影響について検討した。その結果を表10及び図9に示す。
ヒアルロン酸(株式会社資生堂製、バイオヒアロ12:重量平均分子量120万)をクエン酸緩衝液(富士フイルム和光純薬株式会社製:pH6.5、イオン強度0.006)中に0.1質量%の含有量となるように添加し、ボルテックスミキサーで攪拌混合して組成物Cを調製した。ヒアルロン酸を溶解させた後、塩のイオン強度が、0.03、0.06、及び0.30となるように、分取した各組成物Cに対し、クエン酸ナトリウムを添加し、ボルテックスミキサーで攪拌混合してヒアルロン酸粒子含有組成物を各々調製した。ここで、イオン強度が0.03のときのクエン酸ナトリウムの濃度は、0.005Mであり、イオン強度が0.06のときのクエン酸ナトリウムの濃度は、0.010Mであり、イオン強度が0.30のときのクエン酸ナトリウムの濃度は、0.050Mであった。
表10及び図9の結果から明らかなように、塩化ナトリウム以外の塩であっても、200nm以下のヒアルロン酸粒子が得られることが確認できた。
参考試験例6から、水素結合を阻害する添加剤である尿素の使用に伴うヒアルロン酸粒子の粒子径の影響について検討した。その結果を表11及び図10に示す。
ヒアルロン酸(資生堂株式会社製、バイオヒアロ12:重量平均分子量120万)をイオン交換水中に0.1質量%の含有量となるように添加し、ボルテックスミキサーで攪拌混合して組成物Dを調製した。ヒアルロン酸を溶解させた後、塩のイオン強度が0.10となるように、組成物Dに対し、塩化ナトリウムを0.10Mの濃度で添加し、ボルテックスミキサーで攪拌混合してヒアルロン酸粒子含有組成物を調製した。
ヒアルロン酸(資生堂株式会社製、バイオヒアロ12:重量平均分子量120万)を等張のリン酸緩衝液(タカラバイオ株式会社製:pH7.4、イオン強度0.154)中に0.1質量%の含有量となるように添加し、ボルテックスミキサーで攪拌混合してヒアルロン酸粒子含有組成物を調製した。
参考実施例1のヒアルロン酸粒子含有組成物の全量に対し、尿素を10質量%配合して参考比較例1の組成物を調製した。
参考実施例2のヒアルロン酸粒子含有組成物の全量に対し、尿素を10質量%配合して参考比較例2の組成物を調製した。
表11及び図10の結果より、水素結合を切断する作用を奏する尿素を組成物中に添加すると、ヒアルロン酸粒子の粒子径が大幅に上昇することが確認できた。この結果からも明らかなように、塩を用いて調製したヒアルロン酸粒子は、水素結合を切断する尿素の配合によって粒子径が変動していることから、尿素の影響を受けない架橋結合によって得られるような粒子ではなく、水素結合によって粒子化した粒子であると考えられる。
Claims (7)
- 無機塩及び有機酸塩からなる群から選択される少なくとも一種の塩、並びにヒアルロン酸を含む第1剤、並びに、
キレート剤を含む、前記ヒアルロン酸を膨潤させるための第2剤、を含む、
化粧料。 - 前記第1剤中のヒアルロン酸の体積が、前記第1剤に対して前記第2剤を適用すると増大する、請求項1に記載の化粧料。
- 前記ヒアルロン酸が、前記第1剤の全量に対し、0.005質量%以上含まれている、請求項1又は2に記載の化粧料。
- 前記塩を構成する陽イオンが、金属イオンである、請求項1~3のいずれか一項に記載の化粧料。
- 前記キレート剤が、エチレンジアミン四酢酸、エチレンジアミン四酢酸二ナトリウム、エチレンジアミン四酢酸三ナトリウム、ニトリロ三酢酸、ニトリロ三酢酸ナトリウム、ニトリロ三酢酸アンモニウム、ヒドロキシエチルエチレンジアミン三酢酸、ヒドロキシエチルエチレンジアミン三酢酸ナトリウム、ペンテト酸、ペンテト酸五ナトリウム、トリエチレンテトラミン六酢酸、トリエチレンテトラミン六酢酸ナトリウム、イミジコハク酸、イミジコハク酸四ナトリウム、エチレンジアミン二コハク酸、エチレンジアミン二コハク酸三ナトリウム、ヒドロキシエチルイミノ二酢酸、ヒドロキシエチルイミノ二酢酸二ナトリウム、イミノ二コハク酸、イミノ二コハク酸四ナトリウム、トリエチレンテトラミン六酢酸、トリエチレンテトラミン六酢酸ナトリウム、メチルグリシン二酢酸、メチルグリシン二酢酸三ナトリウム、ヒドロキシイミノジコハク酸、ヒドロキシイミノジコハク酸四ナトリウム、L-アスパラギン酸二酢酸L-アスパラギン酸二酢酸四ナトリウム、グルタミン酸ジ酢酸、グルタミン酸ジ酢酸四ナトリウム、プロパンジアミン四酢酸、エチレンジアミン四酢酸二アンモニウム、1,3-ジアミノ-2-ヒドロキシプロパン-四酢酸、1,3-ジアミノ-2-ヒドロキシプロパン-四酢酸、N,N-ビス(2-ヒドロキシエチル)グリシン、グリコールエーテルジアミン四酢酸、二カルボキシメチルグルタミン酸、二カルボキシメチルグルタミン酸四ナトリウム、ヘキサメタリン酸、ジエチレントリアミン五酢酸、ヘキサメタリン酸ナトリウム、ニトリロトリス(メチレンホスホン酸)、ニトリロトリス(メチレンホスホン酸)カリウム、2-ホスホノブタン-1,2,4-トリカルボン酸、エチレンジアミンテトラメチレンホスホン酸、エチレンジアミンテトラメチレンホスホン酸五ナトリウム、フィチン酸、及びクエン酸からなる群から選択される少なくとも一種である、請求項1~4のいずれか一項に記載の化粧料。
- 前記ヒアルロン酸の重量平均分子量が、10,000,000以下である、請求項1~5のいずれか一項に記載の化粧料。
- 請求項1~6のいずれか一項に記載の化粧料を使用する美容方法であって、
前記第1剤を体表又は体毛に適用した後に、当該第1剤の適用面に対して前記第2剤を適用する、
美容方法。
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WO2018182003A1 (ja) | 2017-03-30 | 2018-10-04 | 株式会社 資生堂 | ヒアルロン酸複合ナノ粒子 |
WO2021033725A1 (ja) * | 2019-08-21 | 2021-02-25 | 株式会社 資生堂 | 化粧料 |
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US20240065962A1 (en) | 2024-02-29 |
EP4292582A1 (en) | 2023-12-20 |
TW202245732A (zh) | 2022-12-01 |
JPWO2022172790A1 (ja) | 2022-08-18 |
CN116782867A (zh) | 2023-09-19 |
KR20230137305A (ko) | 2023-10-04 |
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