JP5873264B2 - Oil-in-water emulsion - Google Patents
Oil-in-water emulsion Download PDFInfo
- Publication number
- JP5873264B2 JP5873264B2 JP2011150794A JP2011150794A JP5873264B2 JP 5873264 B2 JP5873264 B2 JP 5873264B2 JP 2011150794 A JP2011150794 A JP 2011150794A JP 2011150794 A JP2011150794 A JP 2011150794A JP 5873264 B2 JP5873264 B2 JP 5873264B2
- Authority
- JP
- Japan
- Prior art keywords
- oil
- viscosity
- water emulsion
- component
- hyaluronic acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000007764 o/w emulsion Substances 0.000 title claims description 47
- -1 hyaluronic acid salt Chemical class 0.000 claims description 42
- 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 description 35
- 229920002674 hyaluronan Polymers 0.000 claims description 32
- 229960003160 hyaluronic acid Drugs 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 25
- 239000004094 surface-active agent Substances 0.000 claims description 25
- 239000001913 cellulose Substances 0.000 claims description 18
- 229920002678 cellulose Polymers 0.000 claims description 18
- 150000003839 salts Chemical class 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 description 23
- 239000000194 fatty acid Substances 0.000 description 17
- 239000003921 oil Substances 0.000 description 17
- 235000014113 dietary fatty acids Nutrition 0.000 description 16
- 229930195729 fatty acid Natural products 0.000 description 16
- 235000019198 oils Nutrition 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 13
- 239000007864 aqueous solution Substances 0.000 description 12
- 239000000203 mixture Substances 0.000 description 10
- 239000012071 phase Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 150000004665 fatty acids Chemical class 0.000 description 9
- 238000000926 separation method Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 229920001296 polysiloxane Polymers 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 230000032683 aging Effects 0.000 description 5
- 239000002736 nonionic surfactant Substances 0.000 description 5
- 239000004006 olive oil Substances 0.000 description 5
- 235000008390 olive oil Nutrition 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 229920002385 Sodium hyaluronate Polymers 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- 235000021317 phosphate Nutrition 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229940010747 sodium hyaluronate Drugs 0.000 description 4
- YWIVKILSMZOHHF-QJZPQSOGSA-N sodium;(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- Chemical compound [Na+].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 YWIVKILSMZOHHF-QJZPQSOGSA-N 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 3
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 239000002280 amphoteric surfactant Substances 0.000 description 3
- 239000003945 anionic surfactant Substances 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 3
- 229960003237 betaine Drugs 0.000 description 3
- 239000003093 cationic surfactant Substances 0.000 description 3
- 239000002537 cosmetic Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000003925 fat Substances 0.000 description 3
- 235000019197 fats Nutrition 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 2
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 2
- WNWHHMBRJJOGFJ-UHFFFAOYSA-N 16-methylheptadecan-1-ol Chemical compound CC(C)CCCCCCCCCCCCCCCO WNWHHMBRJJOGFJ-UHFFFAOYSA-N 0.000 description 2
- XDOFQFKRPWOURC-UHFFFAOYSA-N 16-methylheptadecanoic acid Chemical compound CC(C)CCCCCCCCCCCCCCC(O)=O XDOFQFKRPWOURC-UHFFFAOYSA-N 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N Caprylic acid Natural products CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 2
- 206010040880 Skin irritation Diseases 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 235000018936 Vitellaria paradoxa Nutrition 0.000 description 2
- 150000005215 alkyl ethers Chemical class 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 2
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- NOPFSRXAKWQILS-UHFFFAOYSA-N docosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCO NOPFSRXAKWQILS-UHFFFAOYSA-N 0.000 description 2
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000010696 ester oil Substances 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000036556 skin irritation Effects 0.000 description 2
- 231100000475 skin irritation Toxicity 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- PRAKJMSDJKAYCZ-UHFFFAOYSA-N squalane Chemical compound CC(C)CCCC(C)CCCC(C)CCCCC(C)CCCC(C)CCCC(C)C PRAKJMSDJKAYCZ-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 239000001993 wax Substances 0.000 description 2
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 description 1
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- BODMYPYTCKYRSP-UHFFFAOYSA-N 1,1-dioctylcyclohexane Chemical compound CCCCCCCCC1(CCCCCCCC)CCCCC1 BODMYPYTCKYRSP-UHFFFAOYSA-N 0.000 description 1
- QMMJWQMCMRUYTG-UHFFFAOYSA-N 1,2,4,5-tetrachloro-3-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=C(Cl)C(Cl)=CC(Cl)=C1Cl QMMJWQMCMRUYTG-UHFFFAOYSA-N 0.000 description 1
- 229940058015 1,3-butylene glycol Drugs 0.000 description 1
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 description 1
- DEMBLPGWNXUBIQ-UHFFFAOYSA-N 2-dodecylhexadecan-1-ol Chemical compound CCCCCCCCCCCCCCC(CO)CCCCCCCCCCCC DEMBLPGWNXUBIQ-UHFFFAOYSA-N 0.000 description 1
- LEEDMQGKBNGPDN-UHFFFAOYSA-N 2-methylnonadecane Chemical compound CCCCCCCCCCCCCCCCCC(C)C LEEDMQGKBNGPDN-UHFFFAOYSA-N 0.000 description 1
- LEACJMVNYZDSKR-UHFFFAOYSA-N 2-octyldodecan-1-ol Chemical compound CCCCCCCCCCC(CO)CCCCCCCC LEACJMVNYZDSKR-UHFFFAOYSA-N 0.000 description 1
- OYRKAUXRSTZVFT-UHFFFAOYSA-N 2-octyldodecyl 2,2-dimethyloctanoate Chemical compound CCCCCCCCCCC(CCCCCCCC)COC(=O)C(C)(C)CCCCCC OYRKAUXRSTZVFT-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- UIVPNOBLHXUKDX-UHFFFAOYSA-N 3,5,5-trimethylhexyl 3,5,5-trimethylhexanoate Chemical compound CC(C)(C)CC(C)CCOC(=O)CC(C)CC(C)(C)C UIVPNOBLHXUKDX-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 235000019489 Almond oil Nutrition 0.000 description 1
- 235000021357 Behenic acid Nutrition 0.000 description 1
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 1
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- XMSXQFUHVRWGNA-UHFFFAOYSA-N Decamethylcyclopentasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XMSXQFUHVRWGNA-UHFFFAOYSA-N 0.000 description 1
- LVGKNOAMLMIIKO-UHFFFAOYSA-N Elaidinsaeure-aethylester Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC LVGKNOAMLMIIKO-UHFFFAOYSA-N 0.000 description 1
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Natural products NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- CMBYOWLFQAFZCP-UHFFFAOYSA-N Hexyl dodecanoate Chemical compound CCCCCCCCCCCC(=O)OCCCCCC CMBYOWLFQAFZCP-UHFFFAOYSA-N 0.000 description 1
- 239000004166 Lanolin Substances 0.000 description 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- 235000018330 Macadamia integrifolia Nutrition 0.000 description 1
- 240000000912 Macadamia tetraphylla Species 0.000 description 1
- 235000003800 Macadamia tetraphylla Nutrition 0.000 description 1
- HVVJUIVBAXJULQ-UHFFFAOYSA-N N=C=O.N=C=O.OCC(O)CO Chemical compound N=C=O.N=C=O.OCC(O)CO HVVJUIVBAXJULQ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 235000019483 Peanut oil Nutrition 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- GCSPRLPXTPMSTL-IBDNADADSA-N [(2s,3r,4s,5s,6r)-2-[(2s,3s,4s,5r)-3,4-dihydroxy-2,5-bis(hydroxymethyl)oxolan-2-yl]-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[C@@]1([C@]2(CO)[C@H]([C@H](O)[C@@H](CO)O2)O)O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O GCSPRLPXTPMSTL-IBDNADADSA-N 0.000 description 1
- JAWMENYCRQKKJY-UHFFFAOYSA-N [3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-ylmethyl)-1-oxa-2,8-diazaspiro[4.5]dec-2-en-8-yl]-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]methanone Chemical compound N1N=NC=2CN(CCC=21)CC1=NOC2(C1)CCN(CC2)C(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F JAWMENYCRQKKJY-UHFFFAOYSA-N 0.000 description 1
- DRRMRHKHTQRWMB-UHFFFAOYSA-N [3-(2-ethylhexanoyloxy)-2,2-bis(2-ethylhexanoyloxymethyl)propyl] 2-ethylhexanoate Chemical compound CCCCC(CC)C(=O)OCC(COC(=O)C(CC)CCCC)(COC(=O)C(CC)CCCC)COC(=O)C(CC)CCCC DRRMRHKHTQRWMB-UHFFFAOYSA-N 0.000 description 1
- 230000021736 acetylation Effects 0.000 description 1
- 238000006640 acetylation reaction Methods 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 1
- 239000008168 almond oil Substances 0.000 description 1
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 1
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- 229940077388 benzenesulfonate Drugs 0.000 description 1
- WMNULTDOANGXRT-UHFFFAOYSA-N bis(2-ethylhexyl) butanedioate Chemical compound CCCCC(CC)COC(=O)CCC(=O)OCC(CC)CCCC WMNULTDOANGXRT-UHFFFAOYSA-N 0.000 description 1
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- XHRPOTDGOASDJS-UHFFFAOYSA-N cholesterol n-octadecanoate Natural products C12CCC3(C)C(C(C)CCCC(C)C)CCC3C2CC=C2C1(C)CCC(OC(=O)CCCCCCCCCCCCCCCCC)C2 XHRPOTDGOASDJS-UHFFFAOYSA-N 0.000 description 1
- XHRPOTDGOASDJS-XNTGVSEISA-N cholesteryl stearate Chemical compound C([C@@H]12)C[C@]3(C)[C@@H]([C@H](C)CCCC(C)C)CC[C@H]3[C@@H]1CC=C1[C@]2(C)CC[C@H](OC(=O)CCCCCCCCCCCCCCCCC)C1 XHRPOTDGOASDJS-XNTGVSEISA-N 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- LVGKNOAMLMIIKO-QXMHVHEDSA-N ethyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC LVGKNOAMLMIIKO-QXMHVHEDSA-N 0.000 description 1
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- 239000003205 fragrance Substances 0.000 description 1
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- 238000010438 heat treatment Methods 0.000 description 1
- IUJAMGNYPWYUPM-UHFFFAOYSA-N hentriacontane Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCC IUJAMGNYPWYUPM-UHFFFAOYSA-N 0.000 description 1
- SFFVATKALSIZGN-UHFFFAOYSA-N hexadecan-7-ol Chemical compound CCCCCCCCCC(O)CCCCCC SFFVATKALSIZGN-UHFFFAOYSA-N 0.000 description 1
- DWMMZQMXUWUJME-UHFFFAOYSA-N hexadecyl octanoate Chemical compound CCCCCCCCCCCCCCCCOC(=O)CCCCCCC DWMMZQMXUWUJME-UHFFFAOYSA-N 0.000 description 1
- 229940100463 hexyl laurate Drugs 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
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- 238000002955 isolation Methods 0.000 description 1
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
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- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
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- BJEPYKJPYRNKOW-UHFFFAOYSA-N malic acid Chemical compound OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
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- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 description 1
- 229940078812 myristyl myristate Drugs 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- JXTPJDDICSTXJX-UHFFFAOYSA-N n-Triacontane Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCC JXTPJDDICSTXJX-UHFFFAOYSA-N 0.000 description 1
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000010466 nut oil Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- KSCKTBJJRVPGKM-UHFFFAOYSA-N octan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCCCCCC[O-].CCCCCCCC[O-].CCCCCCCC[O-].CCCCCCCC[O-] KSCKTBJJRVPGKM-UHFFFAOYSA-N 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 229940055577 oleyl alcohol Drugs 0.000 description 1
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 1
- 239000008385 outer phase Substances 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 229920000223 polyglycerol Polymers 0.000 description 1
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- NEOZOXKVMDBOSG-UHFFFAOYSA-N propan-2-yl 16-methylheptadecanoate Chemical compound CC(C)CCCCCCCCCCCCCCC(=O)OC(C)C NEOZOXKVMDBOSG-UHFFFAOYSA-N 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000010667 rosehip oil Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 229940032094 squalane Drugs 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 229940104261 taurate Drugs 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- BORJONZPSTVSFP-UHFFFAOYSA-N tetradecyl 2-hydroxypropanoate Chemical compound CCCCCCCCCCCCCCOC(=O)C(C)O BORJONZPSTVSFP-UHFFFAOYSA-N 0.000 description 1
- DZKXJUASMGQEMA-UHFFFAOYSA-N tetradecyl tetradecanoate Chemical compound CCCCCCCCCCCCCCOC(=O)CCCCCCCCCCCCC DZKXJUASMGQEMA-UHFFFAOYSA-N 0.000 description 1
- PUVAFTRIIUSGLK-UHFFFAOYSA-M trimethyl(oxiran-2-ylmethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC1CO1 PUVAFTRIIUSGLK-UHFFFAOYSA-M 0.000 description 1
- 229940026256 trioctyldodecyl citrate Drugs 0.000 description 1
- BIEMOBPNIWQLMF-UHFFFAOYSA-N tris(2-octyldodecyl) 2-hydroxypropane-1,2,3-tricarboxylate Chemical compound CCCCCCCCCCC(CCCCCCCC)COC(=O)CC(O)(C(=O)OCC(CCCCCCCC)CCCCCCCCCC)CC(=O)OCC(CCCCCCCC)CCCCCCCCCC BIEMOBPNIWQLMF-UHFFFAOYSA-N 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 239000004711 α-olefin Substances 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
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
- A61K8/062—Oil-in-water emulsions
-
- 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
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/731—Cellulose; Quaternized cellulose derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
- A61Q5/02—Preparations for cleaning the hair
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/54—Polymers characterized by specific structures/properties
- A61K2800/542—Polymers characterized by specific structures/properties characterized by the charge
- A61K2800/5426—Polymers characterized by specific structures/properties characterized by the charge cationic
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/59—Mixtures
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Animal Behavior & Ethology (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Chemical & Material Sciences (AREA)
- Emergency Medicine (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Dispersion Chemistry (AREA)
- Cosmetics (AREA)
Description
本発明は、水中油型乳化物に関する。 The present invention relates to an oil-in-water emulsion.
従来より、乳化物を調製する場合に、界面活性剤の配合量を低く抑え、水溶性高分子を乳化剤として配合させることが検討されている。 Conventionally, when preparing an emulsion, it has been studied to keep the blending amount of a surfactant low and blend a water-soluble polymer as an emulsifier.
例えば、特許文献1(特開平07−089823号公報)に記載の乳化組成物では、カチオン化セルロースとヒアルロン酸もしくはその塩を配合させることが提案されている。この特許文献1に記載の発明では、特に、系の粘度が低い乳液において、乳化力や安定性を向上させることを課題視している。 For example, in the emulsion composition described in Patent Document 1 (Japanese Patent Application Laid-Open No. 07-089823), it has been proposed to blend cationized cellulose and hyaluronic acid or a salt thereof. In the invention described in Patent Document 1, the problem is to improve emulsifying power and stability, particularly in an emulsion having a low system viscosity.
また、特許文献2(特開平09−301824号公報)に記載の発明では、従来の界面活性剤を使用しない場合であっても、乳化安定性を良好にさせることを課題としており、カチオン化セルロースとヒアルロン酸ナトリウムとからなるポリイオンコンプレックスを含む水相と、油相とが、油中水型(W/O型)に乳化されてなるW/O型乳化組成物を提案している。 Further, in the invention described in Patent Document 2 (Japanese Patent Application Laid-Open No. 09-301824), it is an object to improve the emulsion stability even when a conventional surfactant is not used. And a water phase containing a polyion complex composed of sodium hyaluronate and an oil phase have been proposed to be emulsified in a water-in-oil type (W / O type).
上記特許文献1に記載の乳化組成物では、特に系の粘度が低い乳液において乳化力や安定性が問題となることに着目し、粘度が150cps、180cps、200cpsの実施例や、粘度が810cps、840cpsの比較例等のように、系の粘度が1000cps(=1000mPa・s)未満である低い粘度についてのみ検討している。これによると、系の粘度が高い場合には、乳化は、特別問題視する必要が無いことが示唆されている。 In the emulsified composition described in Patent Document 1, the emulsification power and stability are particularly problematic in emulsions having a low system viscosity. Examples with viscosities of 150 cps, 180 cps, and 200 cps, and viscosities of 810 cps, Only low viscosities in which the viscosity of the system is less than 1000 cps (= 1000 mPa · s), such as a comparative example of 840 cps, are considered. This suggests that emulsification does not need to be a special problem when the viscosity of the system is high.
ところが、水中油型乳化物に関して発明者らが検討研究したところ、系の粘度が高い場合であっても、安定した乳化物が得られない場合があることが新たに見出された。すなわち、カチオン化セルロースとヒアルロン酸もしくはその塩を配合させ、系の粘度が1000mPa・s以上である高い粘度の乳化物の調製を実際に試みたが、低温環境下に置けば水相と油相が分離してしまい、安定した乳化物が得られないことが確認された(例えば、後述する比較例1参照)。 However, as a result of investigations by the inventors on the oil-in-water emulsion, it was newly found that a stable emulsion may not be obtained even when the viscosity of the system is high. In other words, cationized cellulose and hyaluronic acid or a salt thereof were blended, and an attempt was made to prepare a high viscosity emulsion having a system viscosity of 1000 mPa · s or more. It was confirmed that a stable emulsion could not be obtained (see, for example, Comparative Example 1 described later).
なお、上記特許文献2に記載の乳化組成物では、W/O型乳化組成物のみが提案されており、外相が水相であり油滴が水相中に分散した状態であるO/W型乳化組成物については開示するものではない。つまり、本発明が問題としている高い粘度での水中油型乳化物は確認されていない。 In the emulsion composition described in Patent Document 2, only a W / O type emulsion composition has been proposed, and the O / W type in which the outer phase is an aqueous phase and oil droplets are dispersed in the aqueous phase. The emulsified composition is not disclosed. That is, the oil-in-water type emulsion with the high viscosity which is a problem of the present invention has not been confirmed.
本発明は、上述した点に鑑みてなされたものであり、本発明の課題は、粘度が1000mPa・s以上であっても、低温環境下に置くことによる油相分離が抑制される水中油型乳化物を提供することにある。 This invention is made | formed in view of the point mentioned above, and the subject of this invention is an oil-in-water type | mold by which the oil-phase separation by being placed in a low-temperature environment is suppressed, even if a viscosity is 1000 mPa * s or more. It is to provide an emulsion.
本発明者らは、ヒアルロン酸又はアセチル化ヒアルロン酸とカチオン化セルロースが配合された粘度1000mPa・s以上の水中油型乳化物を得るために鋭意検討を行った結果、所定のアルコールの配合により、低温環境下に置いた後に確認される油相の分離が抑えられることを見出し、本発明を完成するに至った。更に、本発明によれば、所定のアルコールの配合によって、高温環境下に置いた後に確認される粘度低下が抑えられることも本発明者らは見出した。 As a result of diligent studies to obtain an oil-in-water emulsion having a viscosity of 1000 mPa · s or more in which hyaluronic acid or acetylated hyaluronic acid and cationized cellulose are blended, The inventors have found that the separation of the oil phase confirmed after being placed in a low temperature environment can be suppressed, and have completed the present invention. Furthermore, according to the present invention, the present inventors have also found that a decrease in viscosity confirmed after placing in a high temperature environment can be suppressed by blending a predetermined alcohol.
すなわち、本発明に係る水中油型乳化物は、粘度が1000mPa・s以上である水中油型乳化物であって、(A)カチオン化セルロース、(B)ヒアルロン酸、ヒアルロン酸の塩、アセチル化ヒアルロン酸、及び、アセチル化ヒアルロン酸の塩よりなる群から選ばれる少なくとも一種、並びに、(C)炭素数5以下のアルコール、が配合されている。 That is, the oil-in-water emulsion according to the present invention is an oil-in-water emulsion having a viscosity of 1000 mPa · s or more, and includes (A) cationized cellulose, (B) hyaluronic acid, a salt of hyaluronic acid, and acetylation. At least one selected from the group consisting of hyaluronic acid and acetylated hyaluronic acid salts, and (C) an alcohol having 5 or less carbon atoms are blended.
「本発明に係る水中油型乳化物の粘度」とは、水中油型乳化物の調製直後に、B形粘度計(株式会社トキメック製)を用いて、25℃で12rpmの条件下で測定した場合において、測定開始後60秒の時点での値をいう(以下、同じ。)。なお、M2ロータ、M3ロータ等の用いるロータは、測定される粘度に応じて適宜選択される。 The “viscosity of the oil-in-water emulsion according to the present invention” was measured immediately after the preparation of the oil-in-water emulsion using a B-type viscometer (manufactured by Tokimec Co., Ltd.) at 25 ° C. under a condition of 12 rpm. In this case, the value at the time point of 60 seconds after the start of measurement (hereinafter the same). Note that the rotor to be used such as the M2 rotor and the M3 rotor is appropriately selected according to the measured viscosity.
本発明に係る水中油型乳化物は、例えば、毛髪処理剤として用いられる。 The oil-in-water emulsion according to the present invention is used, for example, as a hair treatment agent.
本発明に係る水中油型乳化物は、界面活性剤の配合量が10質量%未満のものが良く、界面活性剤の配合量が5.0質量%未満のものが好ましく、界面活性剤が配合されていないものがより好ましい。皮膚の状況などにより個人差があるが、界面活性剤が配合されていると皮膚に刺激を与える場合があるので、界面活性剤の配合量は10質量%未満とするか、界面活性剤を配合しないのが望ましい。 The oil-in-water emulsion according to the present invention preferably has a surfactant content of less than 10% by mass, preferably has a surfactant content of less than 5.0% by mass, and contains a surfactant. What is not done is more preferable. Although there are individual differences depending on the condition of the skin, etc., if a surfactant is blended, it may irritate the skin, so the blending amount of the surfactant should be less than 10% by mass or blended with a surfactant It is desirable not to.
本発明に係る水中油型乳化物は、[(B)ヒアルロン酸、ヒアルロン酸の塩、アセチル化ヒアルロン酸、及び、アセチル化ヒアルロン酸の塩の総配合量]/[(A)カチオン化セルロースの配合量]で算出される比(B)/(A)が、0.04以上0.32以下のものが好適である。 The oil-in-water emulsion according to the present invention comprises [(B) total blending amount of hyaluronic acid, hyaluronic acid salt, acetylated hyaluronic acid, and acetylated hyaluronic acid salt] / [(A) cationized cellulose The ratio (B) / (A) calculated by “blending amount” is preferably 0.04 or more and 0.32 or less.
本発明の水中油型乳化物は、粘度が1000mPa・s以上であるが、低温環境下に置いても油相分離が抑えられる。 The oil-in-water emulsion of the present invention has a viscosity of 1000 mPa · s or more, but oil phase separation can be suppressed even when placed in a low temperature environment.
本発明の水中油型乳化物は、カチオン化セルロースと、ヒアルロン酸、ヒアルロン酸の塩、アセチル化ヒアルロン酸、及び、アセチル化ヒアルロン酸の塩よりなる群から選ばれる少なくとも一種と、炭素数5以下のアルコールと、が配合されており、粘度が1000mPa・s以上である(本発明の水中油型乳化物における水の配合量は、典型的には70質量%以上である。)。
上記の配合されたカチオン化セルロースと、ヒアルロン酸、ヒアルロン酸の塩、アセチル化ヒアルロン酸、及び、アセチル化ヒアルロン酸の塩よりなる群から選ばれる少なくとも一種は、水相に含まれることになる。この水相に油相が分散した乳化物が、本発明の水中油型乳化物である。
The oil-in-water emulsion of the present invention comprises cationized cellulose, at least one selected from the group consisting of hyaluronic acid, a salt of hyaluronic acid, acetylated hyaluronic acid, and a salt of acetylated hyaluronic acid, and 5 or less carbon atoms. And a viscosity of 1000 mPa · s or more (the amount of water in the oil-in-water emulsion of the present invention is typically 70% by mass or more).
At least one selected from the group consisting of the above-described cationized cellulose, hyaluronic acid, a salt of hyaluronic acid, acetylated hyaluronic acid, and a salt of acetylated hyaluronic acid is included in the aqueous phase. The emulsion in which the oil phase is dispersed in the water phase is the oil-in-water emulsion of the present invention.
(1)組成等
(A)成分:カチオン化セルロース
カチオン化セルロースとしては、例えば、ヒドロキシエチルセルロースに塩化グリシジルトリメチルアンモニウムを付加して得られる4級アンモニウム塩の重合体である塩化O−[2−ヒドロキシ−3−(トリメチルアンモニオ)プロピル]ヒドロキシエチルセルロースが挙げられる。当該カチオン化セルロースは市販されており、例えば、ダウ・ケミカル日本社製「UCARE Polymer JR-30M」、東邦化学工業社製「カチナールHC−200」、東邦化学工業社製「カチナールLC−200」が挙げられる。
(1) Component (A) such as composition: cationized cellulose Examples of the cationized cellulose include O- [2-hydroxychloride, which is a polymer of a quaternary ammonium salt obtained by adding glycidyltrimethylammonium chloride to hydroxyethylcellulose. -3- (Trimethylammonio) propyl] hydroxyethylcellulose. The cationized cellulose is commercially available. For example, “UCARE Polymer JR-30M” manufactured by Dow Chemical Japan Co., Ltd., “Kachinal HC-200” manufactured by Toho Chemical Industry Co., Ltd., “Kachinal LC-200” manufactured by Toho Chemical Industry Co., Ltd. Can be mentioned.
カチオン化セルロースは、2質量%水溶液にしたときの粘度が10000mPa・s以上40000mPa・s以下のものを選定すると良く、20000mPa・s以上40000mPa・s以下のものを選定するのが好ましい。この粘度が高くなるほどに、本発明の水中油型乳化物の粘度も高くなる傾向にある。なお、カチオン化セルロースの2質量%水溶液の粘度については、B形粘度計を用いて、25℃、M4ロータ、12rpmの条件で測定開始から60秒後の値を採用する。 As the cationized cellulose, one having a viscosity of 10,000 mPa · s or more and 40000 mPa · s or less, preferably 20000 mPa · s or more and 40,000 mPa · s or less is preferable when it is made into a 2% by mass aqueous solution. The higher the viscosity, the higher the viscosity of the oil-in-water emulsion of the present invention. In addition, about the viscosity of 2 mass% aqueous solution of cationized cellulose, the value 60 second after a measurement start is employ | adopted on 25 degreeC, M4 rotor, and 12 rpm conditions using a B-type viscosity meter.
カチオン化セルロースのカチオン化度(カチオン化セルロースにおける窒素含有質量の百分率)は、特に限定されないが、1.3%以上2.0%以下が良く、1.5%以上2.0%以下が好ましい。
(A)成分の水中油型乳化物における配合量の下限は、0.20質量%が好ましく、0.25質量%がより好ましい。また、その上限値は、特に限定されないが、水中油型乳化物を高価としないために、0.55質量%が好ましい。
The degree of cationization of the cationized cellulose (percentage of nitrogen-containing mass in the cationized cellulose) is not particularly limited, but is preferably 1.3% or more and 2.0% or less, and preferably 1.5% or more and 2.0% or less. .
The lower limit of the amount of component (A) in the oil-in-water emulsion is preferably 0.20% by mass, and more preferably 0.25% by mass. Moreover, the upper limit is not particularly limited, but is preferably 0.55% by mass in order not to make the oil-in-water emulsion expensive.
(B)成分:ヒアルロン酸、ヒアルロン酸の塩、アセチル化ヒアルロン酸、及び、アセチル化ヒアルロン酸の塩よりなる群から選ばれる少なくとも一種
塩の形態をとるときの(B)成分としては、例えば、ヒアルロン酸ナトリウム、アセチル化ヒアルロン酸ナトリウムとしてのナトリウム塩となった形態である。
Component (B): As the component (B) when taking the form of at least one salt selected from the group consisting of hyaluronic acid, hyaluronic acid salt, acetylated hyaluronic acid, and acetylated hyaluronic acid salt, This is a form of sodium salt as sodium hyaluronate or acetylated sodium hyaluronate.
ヒアルロン酸を選定する場合、例えば、その1質量%水溶液の粘度が15000mPa・s以上30000mPa・s以下のものが良く、19000mPa・s以上26000mPa・sのものでも良い。ヒアルロン酸を選定する場合と同じく、ヒアルロン酸の塩を選定する場合も、1質量%水溶液の粘度が15000mPa・s以上30000mPa・s以下のものが良く、19000mPa・s以上26000mPa・sのものでも良い。なお、それら1質量%水溶液の粘度については、B形粘度計を用いて、25℃、M4ロータ、12rpmの条件で測定開始から60秒後の値を採用する。 In the case of selecting hyaluronic acid, for example, the 1% by weight aqueous solution may have a viscosity of 15000 mPa · s to 30000 mPa · s, or 19000 mPa · s to 26000 mPa · s. As in the case of selecting hyaluronic acid, the viscosity of a 1% by weight aqueous solution is preferably 15000 mPa · s to 30000 mPa · s, and may be 19000 mPa · s to 26000 mPa · s. . In addition, about the viscosity of these 1 mass% aqueous solution, the value of 60 second after a measurement start is employ | adopted on 25 degreeC, M4 rotor, and 12 rpm conditions using a B-type viscosity meter.
(B)成分の水中油型乳化物における配合量の下限値は、特に限定されないが、0.02質量%が好ましく、0.03質量%がより好ましく、0.05質量%がさらに好ましい。(B)成分の水中油型乳化物における配合量の上限値についても、特に限定されないが、水中油型乳化物を高価としないために、0.20質量%が好ましく、0.15質量%がより好ましい。
(A)成分の配合量に対する(B)成分の配合量の比([(B)ヒアルロン酸、ヒアルロン酸の塩、アセチル化ヒアルロン酸、及び、アセチル化ヒアルロン酸の塩の総配合量]/[(A)カチオン化セルロースの配合量]により算出される比(B)/(A))の下限値は、0.04が好ましく、0.10がより好ましい。また、その上限値としては、0.32が好ましく、0.30がより好ましい。比(B)/(A)が0.04以上0.32以下であれば、水中油型乳化物の製造が容易である。
Although the lower limit of the compounding quantity in the oil-in-water emulsion of (B) component is not specifically limited, 0.02 mass% is preferable, 0.03 mass% is more preferable, 0.05 mass% is further more preferable. The upper limit of the amount of component (B) in the oil-in-water emulsion is not particularly limited, but is preferably 0.20% by mass, and 0.15% by mass in order not to make the oil-in-water emulsion expensive. More preferred.
Ratio of blending amount of component (B) to blending amount of component (A) ([B) Total blending amount of hyaluronic acid, hyaluronic acid salt, acetylated hyaluronic acid, and acetylated hyaluronic acid salt] / [ The lower limit value of the ratio (B) / (A)) calculated by (A) Blending amount of cationized cellulose] is preferably 0.04, and more preferably 0.10. Moreover, as the upper limit, 0.32 is preferable and 0.30 is more preferable. When the ratio (B) / (A) is 0.04 or more and 0.32 or less, it is easy to produce an oil-in-water emulsion.
(C)成分:炭素数5以下のアルコール
本発明の水中油型乳化物においては、(C)成分の配合によって、低温環境下に置いた後の油相の分離が抑制される上に、45℃程度の高温環境下に置いたときの粘度低下が抑制される。
Component (C): Alcohol having 5 or less carbon atoms In the oil-in-water emulsion of the present invention, the blending of the component (C) suppresses separation of the oil phase after being placed in a low-temperature environment. Reduced viscosity when placed in a high temperature environment of about ℃.
(C)成分は、炭素数5以下のアルコールであれば特に限定されないが、一価アルコール、二価アルコール、及び、三価アルコールから選択された一種又は二種以上が好ましく、二価アルコール及び/又は三価アルコールがより好ましい。
この(C)成分としては、例えば、エタノール、グリセリン、エチレングリコール、1,3−ブチレングリコール、及び、1,3−プロパンジオールよりなる群から選ばれる少なくとも一種であってよい。なかでも、低温での経時安定性に優れる点で、グリセリン、1,3−プロパンジオールが好ましい。
The component (C) is not particularly limited as long as it is an alcohol having 5 or less carbon atoms, but is preferably one or two or more selected from monohydric alcohols, dihydric alcohols, and trihydric alcohols. Or a trihydric alcohol is more preferable.
The component (C) may be at least one selected from the group consisting of ethanol, glycerin, ethylene glycol, 1,3-butylene glycol, and 1,3-propanediol, for example. Of these, glycerin and 1,3-propanediol are preferable because they are excellent in stability over time at low temperatures.
水中油型乳化物における(C)成分の配合量の下限値は、3.0質量%が好ましく、5.0質量%がより好ましい。その上限値は、15質量%が好ましく、10質量%がより好ましい。 The lower limit of the amount of component (C) in the oil-in-water emulsion is preferably 3.0% by mass, and more preferably 5.0% by mass. The upper limit is preferably 15% by mass, and more preferably 10% by mass.
(D)成分:油相成分
(D)成分は、水との相溶性が無いか又は水との相溶性が低いものであり、本発明の水中油型乳化物の水相中に分散させるものである。(D)成分としては、例えば、25℃で液体又は固体の油脂、エステル油、高級アルコール、ロウ、炭化水素、高級脂肪酸、シリコーンが挙げられる((D)成分の具体例は、株式会社薬事日報社から発行されている「日本化粧品原料集2007」などに記載されている。)。(D)成分は、一種又は二種以上が配合されると良い。
Component (D): Oil phase component Component (D) is not compatible with water or has low compatibility with water, and is dispersed in the water phase of the oil-in-water emulsion of the present invention. It is. Examples of the component (D) include oils and fats, ester oils, higher alcohols, waxes, hydrocarbons, higher fatty acids, and silicones that are liquid or solid at 25 ° C. (Specific examples of the component (D) include: It is described in “Japan Cosmetics Raw Materials 2007” published by the company). (D) A component is good to mix | blend 1 type, or 2 or more types.
(D)成分である油脂としては、例えば、アーモンド油、アボガド油、オリーブ油、シア脂、シア脂油、水添オリーブ油、ステアリルエステルズ、月見草油、チャボトケイソウ種子油、ツバキ油、ババス油、ピーナッツ油、マカデミアナッツ油、野菜油、ローズヒップ油が挙げられる。 Examples of the fats and oils as component (D) include almond oil, avocado oil, olive oil, shea fat, shea fat oil, hydrogenated olive oil, stearyl esters, evening primrose oil, chabodia seed oil, camellia oil, babas oil, peanut oil , Macadamia nut oil, vegetable oil, rosehip oil.
(D)成分であるエステル油としては、例えば、オクタン酸セチル、イソノナン酸イソノニル、セバシン酸ジエチル、ラウリン酸ヘキシル、オレイン酸エチル、ミリスチン酸ミリスチル、ステアリン酸ブチル、イソステアリン酸イソプロピル、2−エチルヘキサン酸セチル、ジ2−エチルヘキサン酸エチレングリコール、ジ(カプリル・カプリン酸)プロピレングリコール、テトラ2−エチルヘキサン酸ペンタエリスリトール、ジメチルオクタン酸2−オクチルドデシル、乳酸ミリスチル、クエン酸トリオクチルドデシル、リンゴ酸ジイソステアリル、コハク酸ジ2−エチルヘキシル、ステアリン酸コレステリルが挙げられる。 Examples of the ester oil as component (D) include cetyl octanoate, isononyl isononanoate, diethyl sebacate, hexyl laurate, ethyl oleate, myristyl myristate, butyl stearate, isopropyl isostearate, and 2-ethylhexanoic acid. Cetyl, ethylene glycol di-2-ethylhexanoate, propylene glycol di (capryl / capric acid), pentaerythritol tetra-2-ethylhexanoate, 2-octyldodecyl dimethyloctanoate, myristyl lactate, trioctyldodecyl citrate, diacid malate Examples include isostearyl, di-2-ethylhexyl succinate, and cholesteryl stearate.
(D)成分である高級アルコールとしては、例えば、セチルアルコール、ステアリルアルコール、アラキルアルコール、ベヘニルアルコール、オレイルアルコール、ヘキシルデカノール、オクチルドデカノール、イソセチルアルコール、ドデシルヘキサデカノール、イソステアリルアルコール、テトラデシルオクタデカノールが挙げられる。 Examples of the higher alcohol as component (D) include cetyl alcohol, stearyl alcohol, aralkyl alcohol, behenyl alcohol, oleyl alcohol, hexyl decanol, octyldodecanol, isocetyl alcohol, dodecyl hexadecanol, isostearyl alcohol, tetradecyl octa A decanol is mentioned.
(D)成分であるロウとしては、例えば、水添オリーブ油ラウリルエステルズ、水添オリーブ油ミリスチルエステルズ、水添オリーブ油セチルエステルズ、ミツロウ、モクロウ、ホホバ油、キャンデリラロウ、カルナウバロウが挙げられる。 Examples of the wax that is component (D) include hydrogenated olive oil lauryl esters, hydrogenated olive oil myristyl esters, hydrogenated olive oil cetyl esters, beeswax, mole, jojoba oil, candelilla wax, and carnauba wax.
(D)成分である炭化水素としては、例えば、ジオクチルシクロヘキサン、軽質流動イソパラフィン、スクワランが挙げられる。 Examples of the hydrocarbon (D) include dioctylcyclohexane, light liquid isoparaffin, and squalane.
(D)成分である高級脂肪酸としては、例えば、イソステアリン酸、オレイン酸、ステアリン酸、パルミチン酸、ベヘン酸、ミリスチン酸、ラノリン脂肪酸、リノール酸が挙げられる。 Examples of the higher fatty acid (D) include isostearic acid, oleic acid, stearic acid, palmitic acid, behenic acid, myristic acid, lanolin fatty acid, and linoleic acid.
(D)成分であるシリコーンとしては、例えば、ジメチルシリコーン(メチルポリシロキサン、高重合メチルポリシロキサン等)、メチルフェニルシリコーン、環状ジメチルシリコーン(オクタメチルシクロテトラシロキサン、デカメチルシクロペンタシロキサン等)、アミノ変性シリコーン(アミノエチルアミノプロピルシロキサン・ジメチルシロキサン共重合体、アミノエチルアミノプロピルメチルシロキサン・ジメチルシロキサン共重合体等)、ポリエーテル変性シリコーン、長鎖アルキル変性シリコーン、シラノール変性シリコーンが挙げられる。 Examples of the silicone as component (D) include dimethyl silicone (methylpolysiloxane, highly polymerized methylpolysiloxane, etc.), methylphenylsilicone, cyclic dimethylsilicone (octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, etc.), amino Examples include modified silicone (aminoethylaminopropylsiloxane / dimethylsiloxane copolymer, aminoethylaminopropylmethylsiloxane / dimethylsiloxane copolymer, etc.), polyether-modified silicone, long-chain alkyl-modified silicone, and silanol-modified silicone.
(D)成分の水中油型乳化物における配合量は、特に限定されないが、例えば、0.5質量%以上15質量%以下である。 Although the compounding quantity in the oil-in-water emulsion of (D) component is not specifically limited, For example, they are 0.5 mass% or more and 15 mass% or less.
(E)成分:任意成分
本発明の水中油型乳化物には、界面活性剤、防腐剤、香料等の公知の毛髪処理剤原料がさらに配合されていてもよい。
(E) Component: Optional component The oil-in-water emulsion of the present invention may further contain a known hair treatment agent material such as a surfactant, preservative, and fragrance.
本発明の水中油型乳化物は、当該乳化物を製造する際の界面活性剤が低配合量又は界面活性剤を配合しないものであり、界面活性剤の配合は、任意となる。本発明の水中油型乳化物に界面活性剤を配合する場合には、ノニオン界面活性剤、カチオン界面活性剤、アニオン界面活性剤、及び、両性界面活性剤の一種又は二種以上を任意に配合する。
水中油型乳化物に界面活性剤(ノニオン界面活性剤、カチオン界面活性剤、アニオン界面活性剤、及び、両性界面活性剤の一種又は二種以上)を配合する場合、その配合量は、使用者に与える皮膚刺激を抑制するために、10質量%未満が好ましく、5.0質量%未満がより好ましく、1.0質量%未満がさらに好ましく、0.5質量%未満が特に好ましい。なお、使用者に与える皮膚刺激を抑制するには、界面活性剤を配合しないことが最適である。
In the oil-in-water emulsion of the present invention, the surfactant in producing the emulsion is a low blending amount or a surfactant is not blended, and the blending of the surfactant is arbitrary. When a surfactant is added to the oil-in-water emulsion of the present invention, any one or more of nonionic surfactant, cationic surfactant, anionic surfactant, and amphoteric surfactant are optionally added. To do.
When blending a surfactant (one or two or more of nonionic surfactant, cationic surfactant, anionic surfactant, and amphoteric surfactant) in an oil-in-water emulsion, the blending amount is the user In order to suppress skin irritation applied to the skin, it is preferably less than 10% by mass, more preferably less than 5.0% by mass, further preferably less than 1.0% by mass, and particularly preferably less than 0.5% by mass. In order to suppress skin irritation given to the user, it is optimal not to add a surfactant.
上記ノニオン界面活性剤としては、例えば、ショ糖脂肪酸エステル(ラウリン酸スクロース等)、ポリオキシエチレンソルビットテトラ脂肪酸エステル(テトラオレイン酸ポリオキシエチレンソルビット(60E.O.)等)、ポリオキシエチレンアルキルエーテル(ポリオキシエチレンラウリルエーテル(25E.O.)等)、グリセリン脂肪酸エステル(ジイソシアリン酸グリセリン等)、ポリオキシエチレンポリオキシプロピレンアルキルエーテル、ポリオキシエチレン脂肪酸エステル、ポリオキシエチレンソルビタン脂肪酸エステル、アルキルグルコシド、ソルビタン脂肪酸エステル、ポリグリセリン脂肪酸エステルが挙げられる。ノニオン界面活性剤は、一般的に界面活性剤の中でも皮膚に低刺激なので、界面活性剤を配合する場合には、ノニオン界面活性剤を選択するのが好ましい。 Examples of the nonionic surfactant include sucrose fatty acid esters (such as sucrose laurate), polyoxyethylene sorbite tetrafatty acid esters (such as tetraoleic acid polyoxyethylene sorbite (60E.O.)), and polyoxyethylene alkyl ether. (Such as polyoxyethylene lauryl ether (25E.O.)), glycerin fatty acid ester (such as glycerin diisocyanate), polyoxyethylene polyoxypropylene alkyl ether, polyoxyethylene fatty acid ester, polyoxyethylene sorbitan fatty acid ester, alkyl glucoside, Examples include sorbitan fatty acid esters and polyglycerol fatty acid esters. Nonionic surfactants are generally less irritating to the skin among surfactants, and therefore, when blending surfactants, it is preferable to select nonionic surfactants.
上記カチオン界面活性剤としては、例えば、長鎖アルキルトリメチルアンモニウム塩、ジ長鎖アルキルジメチルアンモニウム塩、トリ長鎖アルキルモノメチルアンモニウム塩、ベンザルコニウム型4級アンモニウム塩、モノアルキルエーテル型4級アンモニウム塩が挙げられる。 Examples of the cationic surfactant include a long-chain alkyltrimethylammonium salt, a dilong-chain alkyldimethylammonium salt, a trilong-chain alkylmonomethylammonium salt, a benzalkonium-type quaternary ammonium salt, and a monoalkylether-type quaternary ammonium salt. Is mentioned.
上記アニオン界面活性剤としては、例えば、脂肪酸塩、アルキルエーテルカルボン酸塩、脂肪酸アミドエーテルカルボン酸塩、脂肪酸アミドエーテルカルボン酸、アシル乳酸塩、アルカンスルホン酸塩、α−オレフィンスルホン酸塩、α−スルホ脂肪酸メチルエステル塩、アシルイセチオン酸塩、アルキルグリシジルエーテルスルホン酸塩、アルキルスルホコハク酸塩、アルキルスルホ酢酸塩、アルキルベンゼンスルホン酸塩、アルキルナフタレンスルホン酸塩、N−アシルメチルタウリン塩、アルキル硫酸塩、アルキルエーテル硫酸塩、アルキルアリールエーテル硫酸塩、脂肪酸アルカノールアミド硫酸塩、脂肪酸モノグリセリド硫酸塩、アルキルリン酸塩、ポリオキシエチレンアルキルエーテルリン酸塩、アルキルアリールエーテルリン酸塩、脂肪酸アミドエーテルリン酸塩が挙げられる。 Examples of the anionic surfactant include fatty acid salts, alkyl ether carboxylates, fatty acid amide ether carboxylates, fatty acid amide ether carboxylic acids, acyl lactates, alkane sulfonates, α-olefin sulfonates, α- Sulfo fatty acid methyl ester salt, acyl isethionate, alkyl glycidyl ether sulfonate, alkyl sulfosuccinate, alkyl sulfoacetate, alkyl benzene sulfonate, alkyl naphthalene sulfonate, N-acyl methyl taurate, alkyl sulfate, alkyl Ether sulfate, alkyl aryl ether sulfate, fatty acid alkanolamide sulfate, fatty acid monoglyceride sulfate, alkyl phosphate, polyoxyethylene alkyl ether phosphate, alkyl aryl ether phosphate Examples include salts and fatty acid amide ether phosphates.
上記両性界面活性剤としては、例えば、アルキルグリシン塩、カルボキシメチルグリシン塩、N−アシルアミノエチル−N−2−ヒドロキシエチルグリシン塩、アルキルポリアミノポリカルボキシグリシン塩、アルキルアミノプロピオン酸塩、アルキルイミノジプロピオン酸塩、N−アシルアミノエチル−N−2−ヒドロキシエチルプロピオン酸塩、アルキルジメチルアミノ酢酸ベタイン、脂肪酸アミドプロピルジメチルアミノ酢酸ベタイン、アルキルジヒドロキシエチルアミノ酢酸ベタイン、N−アルキル−N,N−ジメチルアンモニウム−N−プロピルスルホン酸塩、N−アルキル−N,N−ジメチルアンモニウム−N−(2−ヒドロキシプロピル)スルホン酸塩、N−脂肪酸アミドプロピル−N,N−ジメチルアンモニウム−N−(2−ヒドロキシプロピル)スルホン酸塩が挙げられる。 Examples of the amphoteric surfactant include alkyl glycine salt, carboxymethyl glycine salt, N-acylaminoethyl-N-2-hydroxyethyl glycine salt, alkyl polyaminopolycarboxyglycine salt, alkylaminopropionate, alkyliminodi Propionate, N-acylaminoethyl-N-2-hydroxyethylpropionate, alkyldimethylaminoacetic acid betaine, fatty acid amidopropyldimethylaminoacetic acid betaine, alkyldihydroxyethylaminoacetic acid betaine, N-alkyl-N, N-dimethyl Ammonium-N-propylsulfonate, N-alkyl-N, N-dimethylammonium-N- (2-hydroxypropyl) sulfonate, N-fatty acid amidopropyl-N, N-dimethylammonium-N- (2 Hydroxypropyl) sulfonate.
(2)粘度
本発明の水中油型乳化物の粘度は、1000mPa・s以上である。なお、本発明の水中油型乳化物を毛髪処理剤として用いる場合のハンドリング性を考慮すれば、当該水中油型乳化物の粘度は、1500mPa・s以上30000mPa・s以下が良く、2000mPa・s以上20000mPa・s以下が好ましく、2500mPa・s以上10000mPa・s以下がより好ましい。
粘度の調整手法は、例えば、配合される(A)成分又は(B)成分の平均分子量を上げることで(2質量%水溶液の粘度が高い(A)成分を選定又は1質量%水溶液の粘度が高い(B)成分を選定することで)粘度を上げることができ、また、(A)成分及び(B)成分の配合量を多くすることで粘度を上げることができる。また、(A)成分又は(B)成分の平均分子量を下げる(2質量%水溶液の粘度が低い(A)成分を選定又は1質量%水溶液の粘度が低い(B)成分を選定することで)粘度を下げることができ、また、(A)成分及び(B)成分の配合量を少なくすることで粘度を下げることができる。
(2) Viscosity The viscosity of the oil-in-water emulsion of the present invention is 1000 mPa · s or more. In consideration of handling properties when the oil-in-water emulsion of the present invention is used as a hair treatment agent, the viscosity of the oil-in-water emulsion is preferably 1500 mPa · s or more and 30000 mPa · s or less, and 2000 mPa · s or more. 20000 mPa · s or less is preferable, and 2500 mPa · s or more and 10,000 mPa · s or less is more preferable.
For example, the viscosity is adjusted by increasing the average molecular weight of the component (A) or the component (B) (the component (A) having a high viscosity of the 2% by weight aqueous solution is selected or the viscosity of the 1% by weight aqueous solution is The viscosity can be increased by selecting a high (B) component, and the viscosity can be increased by increasing the blending amount of the (A) component and the (B) component. Also, lower the average molecular weight of component (A) or component (B) (by selecting component (A) where the viscosity of the 2% by weight aqueous solution is low or by selecting component (B) where the viscosity of the 1% by weight aqueous solution is low) The viscosity can be lowered, and the viscosity can be lowered by reducing the blending amount of the component (A) and the component (B).
(3)pH
水中油型乳化物のpHは、特に限定されないが、例えば4.0以上9.0以下であり、毛髪処理剤用途として汎用的なのは5.0以上8.0以下である。
(3) pH
The pH of the oil-in-water emulsion is not particularly limited, but is, for example, 4.0 or more and 9.0 or less, and is generally 5.0 or more and 8.0 or less for use as a hair treatment agent.
(4)用途
水中油型乳化物の用途は、特に限定されないが、例えば、毛髪処理剤等の化粧品として用いることができ、界面活性剤を少量配合又は配合しないで洗い流さないトリートメントとして用いてもよい。
(4) Uses The use of the oil-in-water emulsion is not particularly limited. For example, the oil-in-water emulsion can be used as a cosmetic such as a hair treatment agent, and may be used as a treatment in which a small amount of a surfactant is not blended or is not washed away. .
以下、実施例に基づいて本発明を詳細に述べる。ただし、下記実施例は、本発明を限定するものではない。なお、以下の実施例などにおいて、「%」は「質量%」を意味している。また、水中油型乳化物における配合量は、全体で100%となるように各成分の配合量を%で示し、後記の各表中ではその%の表示を省略し、配合量を表す数値のみで表示する。 Hereinafter, the present invention will be described in detail based on examples. However, the following examples do not limit the present invention. In the following examples, “%” means “mass%”. In addition, the blending amount in the oil-in-water emulsion indicates the blending amount of each component in% so that it becomes 100% as a whole, and in the tables below, that percentage is omitted and only the numerical value representing the blending amount Is displayed.
(製造例)
(A)成分の水溶液を調製し、更に(B)成分以外の原料を(A)成分水溶液に配合した(固形原料については加温溶融させて、配合した。)。その(B)成分以外の原料の配合に伴い、白濁するまでホモミキサーを用いて攪拌条件3000rpmで攪拌した。次に、(B)成分の0.33質量%水溶液を配合して、さらにホモミキサーを用いて攪拌することで水中油型乳化物を得た。ここで、ホモミキサーによる攪拌条件は、5000rpmで5分間とした。以上の製造手順により、pHが5.0〜6.0である実施例の水中油型乳化物等を製造した。
(Production example)
An aqueous solution of the component (A) was prepared, and further raw materials other than the component (B) were blended in the aqueous solution of the component (A) (the solid raw material was blended by heating and melting). With the blending of raw materials other than the component (B), the mixture was stirred at 3000 rpm using a homomixer until cloudy. Next, the 0.33 mass% aqueous solution of (B) component was mix | blended, and the oil-in-water emulsion was obtained by further stirring using a homomixer. Here, the stirring condition by the homomixer was 5000 rpm for 5 minutes. The oil-in-water emulsion of the Example whose pH is 5.0-6.0 was manufactured by the above manufacturing procedure.
(評価基準)
乳化物を調製できたか否かの評価(乳化物調製)は、調製後数時間が経過した後、目視によって確認し、以下のように評価した。
○:乳化物として確認できた。
×:分離(透明層と不透明層の存在が明確な状態、以下同じ。)が確認された。
(Evaluation criteria)
Evaluation (emulsion preparation) of whether or not the emulsion could be prepared was confirmed by visual observation after several hours after preparation and evaluated as follows.
○: It was confirmed as an emulsion.
X: Separation (a state in which the presence of a transparent layer and an opaque layer is clear, the same applies hereinafter) was confirmed.
(経時試験)
調製した乳化物等を収容した密栓ガラス管を、下記表1〜4、6に記載の各温度条件における恒温槽内に放置した。外観の経時変化は、目視によって確認し、以下のように評価した。
◎:分離、油の浮き、及び析出物が認められなかった。
○:分離は認められなかったが、僅かに油浮き又は析出物が認められた。
△:分離は認められなかったが、油浮き又は析出物が認められた。
×:分離が認められた。
(Aging test)
The sealed glass tube containing the prepared emulsion and the like was left in a thermostatic bath under each temperature condition described in Tables 1 to 4 and 6 below. The change in appearance over time was confirmed by visual observation and evaluated as follows.
A: Separation, floating of oil, and precipitate were not observed.
○: Separation was not observed, but slight oil floating or deposits were observed.
(Triangle | delta): Although isolation | separation was not recognized, the oil float or deposit was recognized.
X: Separation was observed.
以下、具体的な配合成分や比率を変えながら検討した実施例1−28及び比較例1−8を、表1−6に示す。 Hereinafter, Table 1-2 shows Example 1-28 and Comparative Example 1-8 studied while changing specific blending components and ratios.
以下の表1では、実施例1−7及び比較例1について、経時試験前の初期粘度と、調製後に−10℃の恒温槽内で放置させた後に常温復帰させた際の外観について、放置日数毎に(7日間、18日間、24日間)観察した結果を示す。 In Table 1 below, for Examples 1-7 and Comparative Example 1, the initial viscosity before the aging test and the appearance when the product is allowed to stand in a thermostatic bath at −10 ° C. after preparation are returned to room temperature. The observation results are shown every time (7 days, 18 days, 24 days).
表2では、油相における成分を変えた場合を比較しているが、毛髪処理剤等の化粧品の分野で用いられる油相成分であれば、特に種類を問わず、低温下であっても高温下であっても、水中油型乳化物が安定であったことが確認された。 In Table 2, although the case where the component in an oil phase was changed is compared, if it is an oil phase component used in the field | areas of cosmetics, such as a hair treatment agent, it will be high temperature even if it is low temperature especially if it is a kind. Even underneath, it was confirmed that the oil-in-water emulsion was stable.
表3では、B/Aの値が異なる2つの例について、界面活性剤の有無の違いの影響を検討したが、いずれの実施例16−19についても水中油型乳化物を安定させることができており、特に実施例16、19では界面活性剤を配合しなくても安定性が高いことが確認された。 In Table 3, although the influence of the presence or absence of the surfactant was examined for two examples having different B / A values, the oil-in-water emulsion could be stabilized for any of Examples 16-19. In particular, in Examples 16 and 19, it was confirmed that the stability was high without adding a surfactant.
表4では、配合される界面活性剤の種類によらず、実施例20−23のいずれについても水中油型乳化物を安定させることができることが確認された。 In Table 4, it was confirmed that the oil-in-water emulsion could be stabilized for any of Examples 20-23 regardless of the type of surfactant to be blended.
表5に示すとおり、比較例2は、粘度が1000mPa・sをはるかに超える5260mPa・sであったにもかかわらず、乳化物とならなかったものである。つまり、粘度を単に高めるだけでは乳化物を得ることすらできない。また、表1に示すように、B/Aの値が0.04以上0.32以下の範囲である実施例24−28については、乳化物調製の評価が「○」であったので、B/Aの値が0.04以上0.32以下であれば乳化物調製に適していることが確認された。 As shown in Table 5, Comparative Example 2 did not become an emulsion even though the viscosity was 5260 mPa · s far exceeding 1000 mPa · s. In other words, an emulsion cannot be obtained simply by increasing the viscosity. Further, as shown in Table 1, for Examples 24-28 in which the value of B / A is in the range of 0.04 to 0.32, the evaluation of emulsion preparation was “◯”. When the value of / A was 0.04 or more and 0.32 or less, it was confirmed that it was suitable for emulsion preparation.
上記実施例16と比較例1に関して、以下の表6では、経時試験前の初期粘度と、調製後に45℃の恒温槽内で放置させた後に常温復帰させた際の粘度について放置日数毎(1ヶ月間、2ヶ月間、3ヶ月間)に示す。 With respect to Example 16 and Comparative Example 1, in Table 6 below, the initial viscosity before the time-lapse test and the viscosity when the product is allowed to stand after being prepared in a 45 ° C. constant temperature bath and returned to room temperature are stored every day (1 Month, 2 months, 3 months).
Claims (4)
(A)カチオン化セルロース、
(B)ヒアルロン酸、ヒアルロン酸の塩、アセチル化ヒアルロン酸、及び、アセチル化ヒアルロン酸の塩よりなる群から選ばれる少なくとも一種、並びに、
(C)炭素数5以下のアルコール、
が配合され、
[(B)ヒアルロン酸、ヒアルロン酸の塩、アセチル化ヒアルロン酸、及び、アセチル化ヒアルロン酸の塩の総配合量]/[(A)カチオン化セルロースの配合量]で算出される比(B)/(A)が、0.1以上0.32以下であり、
界面活性剤の配合量が1.0質量%未満、又は、界面活性剤が配合されていない、
水中油型乳化物。 An oil-in-water emulsion having a viscosity of 1000 mPa · s or more,
(A) cationized cellulose,
(B) at least one selected from the group consisting of hyaluronic acid, a salt of hyaluronic acid, acetylated hyaluronic acid, and a salt of acetylated hyaluronic acid, and
(C) an alcohol having 5 or less carbon atoms,
Is blended,
[(B) Total ratio of hyaluronic acid, hyaluronic acid salt, acetylated hyaluronic acid, and acetylated hyaluronic acid salt] / [Ratio calculated by (A) cationized cellulose content] (B) / (A) is 0.1 or more and 0.32 or less,
The blending amount of the surfactant is less than 1.0% by mass, or the surfactant is not blended,
Oil-in-water emulsion.
請求項1に記載の水中油型乳化物。 The blending amount of the surfactant is less than 0.5% by mass, or the surfactant is not blended,
The oil-in-water emulsion according to claim 1.
請求項1または2に記載の水中油型乳化物。 (C) The amount of alcohol having 5 or less carbon atoms is 5.0% by mass or more,
The oil-in-water emulsion according to claim 1 or 2.
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