JP6522408B2 - Water-in-oil emulsified cosmetic - Google Patents
Water-in-oil emulsified cosmetic Download PDFInfo
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- JP6522408B2 JP6522408B2 JP2015089891A JP2015089891A JP6522408B2 JP 6522408 B2 JP6522408 B2 JP 6522408B2 JP 2015089891 A JP2015089891 A JP 2015089891A JP 2015089891 A JP2015089891 A JP 2015089891A JP 6522408 B2 JP6522408 B2 JP 6522408B2
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- titanium oxide
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- ascorbic acid
- cosmetic
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- 239000002537 cosmetic Substances 0.000 title claims description 41
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 66
- MIJPAVRNWPDMOR-ZAFYKAAXSA-N L-ascorbic acid 2-phosphate Chemical compound OC[C@H](O)[C@H]1OC(=O)C(OP(O)(O)=O)=C1O MIJPAVRNWPDMOR-ZAFYKAAXSA-N 0.000 claims description 37
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 36
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 36
- 239000000377 silicon dioxide Substances 0.000 claims description 33
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 5
- 230000000694 effects Effects 0.000 description 15
- 239000002245 particle Substances 0.000 description 14
- 238000011282 treatment Methods 0.000 description 12
- 230000002087 whitening effect Effects 0.000 description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 10
- 238000011156 evaluation Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 230000001681 protective effect Effects 0.000 description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 6
- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- 229910052749 magnesium Inorganic materials 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000011787 zinc oxide Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 206010042496 Sunburn Diseases 0.000 description 4
- 239000006096 absorbing agent Substances 0.000 description 4
- 239000008346 aqueous phase Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000004445 quantitative analysis Methods 0.000 description 4
- 206010014970 Ephelides Diseases 0.000 description 3
- 208000003351 Melanosis Diseases 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000000149 argon plasma sintering Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000004945 emulsification Methods 0.000 description 3
- OSORMYZMWHVFOZ-UHFFFAOYSA-N phenethyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCCC1=CC=CC=C1 OSORMYZMWHVFOZ-UHFFFAOYSA-N 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 239000011164 primary particle Substances 0.000 description 3
- 230000004224 protection Effects 0.000 description 3
- -1 silane compound Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- QNESDXMHQYMNGD-UHFFFAOYSA-N 2,3-bis(3,5,5-trimethylhexanoyloxy)propyl 3,5,5-trimethylhexanoate Chemical compound CC(C)(C)CC(C)CC(=O)OCC(OC(=O)CC(C)CC(C)(C)C)COC(=O)CC(C)CC(C)(C)C QNESDXMHQYMNGD-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229940125904 compound 1 Drugs 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007854 depigmenting agent Substances 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000002250 progressing effect Effects 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 108700004121 sarkosyl Proteins 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 230000000475 sunscreen effect Effects 0.000 description 2
- 239000000516 sunscreening agent Substances 0.000 description 2
- WBYWAXJHAXSJNI-VOTSOKGWSA-M .beta-Phenylacrylic acid Natural products [O-]C(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-M 0.000 description 1
- 229940058015 1,3-butylene glycol Drugs 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241001340526 Chrysoclista linneella Species 0.000 description 1
- WBYWAXJHAXSJNI-SREVYHEPSA-N Cinnamic acid Chemical compound OC(=O)\C=C/C1=CC=CC=C1 WBYWAXJHAXSJNI-SREVYHEPSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 150000000996 L-ascorbic acids Chemical class 0.000 description 1
- 239000004909 Moisturizer Substances 0.000 description 1
- YBGZDTIWKVFICR-JLHYYAGUSA-N Octyl 4-methoxycinnamic acid Chemical compound CCCCC(CC)COC(=O)\C=C\C1=CC=C(OC)C=C1 YBGZDTIWKVFICR-JLHYYAGUSA-N 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 208000012641 Pigmentation disease Diseases 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 206010040829 Skin discolouration Diseases 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- XXBXDAPNXSZAMH-UHFFFAOYSA-N [2,2-dimethyl-3-(3,5,5-trimethylhexanoyloxy)propyl] 3,5,5-trimethylhexanoate Chemical compound CC(C)(C)CC(C)CC(=O)OCC(C)(C)COC(=O)CC(C)CC(C)(C)C XXBXDAPNXSZAMH-UHFFFAOYSA-N 0.000 description 1
- YFCGDEUVHLPRCZ-UHFFFAOYSA-N [dimethyl(trimethylsilyloxy)silyl]oxy-dimethyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C YFCGDEUVHLPRCZ-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000019437 butane-1,3-diol Nutrition 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229930016911 cinnamic acid Natural products 0.000 description 1
- 235000013985 cinnamic acid Nutrition 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000008406 cosmetic ingredient Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- WNLFPMNBHCWASX-UHFFFAOYSA-N dodecyl 2,2-dimethylpropanoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)(C)C WNLFPMNBHCWASX-UHFFFAOYSA-N 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- KWLMIXQRALPRBC-UHFFFAOYSA-L hectorite Chemical compound [Li+].[OH-].[OH-].[Na+].[Mg+2].O1[Si]2([O-])O[Si]1([O-])O[Si]([O-])(O1)O[Si]1([O-])O2 KWLMIXQRALPRBC-UHFFFAOYSA-L 0.000 description 1
- 229910000271 hectorite Inorganic materials 0.000 description 1
- CZWLNMOIEMTDJY-UHFFFAOYSA-N hexyl(trimethoxy)silane Chemical compound CCCCCC[Si](OC)(OC)OC CZWLNMOIEMTDJY-UHFFFAOYSA-N 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 239000004137 magnesium phosphate Substances 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 0.000 description 1
- 235000010270 methyl p-hydroxybenzoate Nutrition 0.000 description 1
- 239000004292 methyl p-hydroxybenzoate Substances 0.000 description 1
- WBYWAXJHAXSJNI-UHFFFAOYSA-N methyl p-hydroxycinnamate Natural products OC(=O)C=CC1=CC=CC=C1 WBYWAXJHAXSJNI-UHFFFAOYSA-N 0.000 description 1
- LXCFILQKKLGQFO-UHFFFAOYSA-N methylparaben Chemical compound COC(=O)C1=CC=C(O)C=C1 LXCFILQKKLGQFO-UHFFFAOYSA-N 0.000 description 1
- 229960002216 methylparaben Drugs 0.000 description 1
- 230000001333 moisturizer Effects 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 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
- 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
- 229960001679 octinoxate Drugs 0.000 description 1
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 1
- 229960003493 octyltriethoxysilane Drugs 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 229940098888 phenethyl benzoate Drugs 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000019612 pigmentation Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 description 1
- 235000010378 sodium ascorbate Nutrition 0.000 description 1
- 229960005055 sodium ascorbate Drugs 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 1
- 229940116962 triisononanoin Drugs 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Landscapes
- Cosmetics (AREA)
Description
本願発明は、アスコルビン酸−２−リン酸塩及び疎水化処理シリカ被覆酸化チタンを安定に含有する化粧料に関する。より詳細には、疎水化処理シリカ被覆酸化チタンを含有しながらもアスコルビン酸−２−リン酸塩の経時安定性が保たれており、紫外線防御効果と美白効果を両立している油中水型乳化化粧料に関する。 The present invention relates to a cosmetic which stably contains ascorbic acid-2-phosphate and hydrophobized silica-coated titanium oxide. More specifically, while containing hydrophobized silica-coated titanium oxide, the stability over time of ascorbic acid-2-phosphate is maintained, and a water-in-oil type in which the ultraviolet light protective effect and the whitening effect are compatible. It relates to an emulsion cosmetic.
日光からの紫外線の刺激により、皮膚のメラニン色素の生成が促されると、しみやそばかすの原因である皮膚の色素沈着が生じる。こうした日焼けによるしみやそばかすを防止するために、美白剤を含有した化粧料が用いられてきた。美白剤としては、優れたメラニン色素生成抑制効果やメラニン色素に対する還元性を示すアスコルビン酸及びその塩並びに誘導体が多く用いられている。アスコルビン酸誘導体の代表としてはアスコルビン酸−２−リン酸塩があり、多くの化粧料に含有されている（特許文献１及び２）。 The stimulation of ultraviolet light from sunlight promotes the formation of melanin pigment in the skin, resulting in pigmentation of the skin, which is the cause of blotches and freckles. In order to prevent such stains and freckles due to sunburn, cosmetics containing a whitening agent have been used. As the skin lightening agent, ascorbic acid and salts and derivatives thereof which exhibit excellent melanin pigment formation inhibitory effect and reducibility to melanin pigment are often used. Ascorbic acid 2-phosphate is a representative of ascorbic acid derivatives, and is contained in many cosmetics (Patent Documents 1 and 2).
しかしながら、アスコルビン酸−２−リン酸塩は日焼け後の美白には効果があるが、紫外線による肌への悪影響を防御する日焼け止めとしての効果はない。このため、美白効果と紫外線防御効果を併せ持つ化粧料が強く望まれていた。 However, although ascorbic acid-2-phosphate is effective for whitening after sunburn, it is not effective as a sunscreen to prevent the adverse effects of ultraviolet rays on the skin. For this reason, a cosmetic having both a whitening effect and an ultraviolet light protection effect has been strongly desired.
従来、化粧料に紫外線防御効果を付与するために、酸化チタンや酸化亜鉛等の無機系紫外線散乱剤やケイ皮酸系等の有機系紫外線吸収剤等が汎用されてきた（非特許文献１〜３）。 Heretofore, inorganic ultraviolet light scattering agents such as titanium oxide and zinc oxide, organic ultraviolet light absorbents such as cinnamic acid, and the like have been widely used in order to impart ultraviolet light protective effects to cosmetics (Non-Patent Documents 1 to 4) 3).
一般的に、高い紫外線防御効果を発揮するために有機系紫外線吸収剤を含有すると、べたつきなどの使用感の悪化につながるため、紫外線散乱剤が併用される。しかしながら、紫外線散乱剤である酸化チタンや酸化亜鉛の表面活性や溶出イオン等によって、アスコルビン酸−２−リン酸塩は酸化されて、褐色に変色してしまい化粧料の外観を著しく損なうとともに、美白効果が低減するという欠点を有する。したがって、アスコルビン酸−２−リン酸塩と紫外線散乱剤を併用することは技術的に困難であった。（特許文献３及び４）。 Generally, when an organic ultraviolet absorber is contained to exhibit a high ultraviolet light protective effect, it leads to deterioration of feeling of use such as stickiness, so that an ultraviolet scattering agent is used in combination. However, ascorbic acid-2-phosphate is oxidized by the surface activity of the ultraviolet light scattering agents such as titanium oxide and zinc oxide, and eluted ions, and it is discolored to brown, and the appearance of the cosmetic is significantly impaired. It has the disadvantage that the effect is reduced. Therefore, it has been technically difficult to use ascorbic acid-2-phosphate in combination with an ultraviolet light scattering agent. (Patent documents 3 and 4).
本願発明における課題は、高い美白効果と紫外線防御効果を両立しながらも、経時的に美白剤が安定に含有されている油中水型乳化化粧料を提供することである。 An object of the present invention is to provide a water-in-oil type emulsion cosmetic which comprises a skin lightening agent stably with time while achieving both a high skin lightening effect and an ultraviolet light protection effect.
かかる事情に鑑み、本願発明者は鋭意研究の結果、疎水化処理シリカ被覆酸化チタンとアスコルビン酸−２−リン酸塩を組み合わせて含有することにより、高い紫外線防御効果により日焼けを防ぐ効果と日焼けによるしみやそばかすを防止する効果を両立しながらも、経時安定性に優れた油中水型乳化化粧料を提供しうることを見出し、本願発明を完成するに至った。 In view of such circumstances, the inventor of the present application has intensively studied, and by combining the hydrophobized silica-coated titanium oxide and ascorbic acid-2-phosphate in combination, the effect of preventing sunburn by a high ultraviolet light protection effect and sunburn It has been found that it is possible to provide a water-in-oil type emulsified cosmetic having excellent stability over time while achieving both the effect of preventing stains and freckles, and to complete the present invention.
すなわち本願発明は、次の成分（Ａ）及び（Ｂ）；
（Ａ）化１で表わされるアスコルビン酸−２−リン酸塩
を含有し、（Ｂ）疎水化処理シリカ被覆酸化チタン中、シリカ被覆量が３０重量％以上であり、疎水化処理剤の含有量が５重量％以上であることを特徴とする油中水型乳化化粧料である。
That is, the present invention comprises the following components (A) and (B):
(A) Ascorbic acid-2-phosphate represented by the formula 1
また、本願発明は、更に、ハンセン溶解度パラメーターδが１７〜２１ＭＰａ０．５の範囲にある油剤を含有することを特徴とする油中水型乳化化粧料である。 Further, the invention of the present application is the water-in-oil type emulsified cosmetic, further comprising an oil agent having a Hansen solubility parameter δ in the range of 17 to 21 MPa 0.5 .
本願発明は、疎水化処理シリカ被覆酸化チタンとアスコルビン酸−２−リン酸塩を含有し、高い紫外線防御効果と美白効果を両立するとともに、アスコルビン酸−２−リン酸塩が経時的に安定に含有されている油中水型乳化化粧料に関する。 The present invention contains hydrophobized silica-coated titanium oxide and ascorbic acid-2-phosphate, and achieves both a high ultraviolet light protective effect and a whitening effect, while ascorbic acid-2-phosphate is stabilized with time. The present invention relates to a water-in-oil type emulsified cosmetic contained.
本願発明で用いられる（Ａ）化１で表わされるアスコルビン酸−２−リン酸塩は、上記化１で表される化合物であって、アスコルビン酸−２−リン酸ナトリウム、アスコルビン酸−２−リン酸マグネシウム、アスコルビン酸−２−リン酸カリウム、アスコルビン酸−２−リン酸カルシウム、アスコルビン酸−２−リン酸アンモニウム等が挙げられるが、これらに限定されるものではない。これらアスコルビン酸−２−リン酸塩の１種又は２種以上を適宜組み合わせて用いることができる。この中でも、水溶性の点からアスコルビン酸−２−リン酸マグネシウム及び／又はアスコルビン酸−２−リン酸ナトリウムが好ましい。 Ascorbic acid-2-phosphate represented by (A) compound 1 used in the present invention is a compound represented by the above-mentioned compound 1, which is sodium ascorbyl 2-phosphate, ascorbic 2-phosphate Examples thereof include, but are not limited to, magnesium acid, potassium ascorbate-2-phosphate, calcium ascorbate-2-phosphate, ammonium ascorbate-2-phosphate and the like. One or two or more of these ascorbic acid-2-phosphates can be used in appropriate combination. Among these, magnesium ascorbyl 2-phosphate and / or sodium ascorbate 2-phosphate are preferable from the viewpoint of water solubility.
本願発明の化粧料において、（Ａ）化１で表わされるアスコルビン酸−２−リン酸塩の含有量は特に限定されないが、化粧料中１〜５重量％含有することが好ましく、より好ましくは２〜４重量％含有されるように用いると良い。含有量が１重量％未満であると十分な美白効果が得られず、５重量％を越えて含有しても美白効果の向上が望めないだけではなく、べたつきや変臭などの問題が生じることがある。 In the cosmetic of the present invention, the content of ascorbic acid-2-phosphate represented by (A) Chemical formula 1 is not particularly limited, but it is preferably contained in an amount of 1 to 5% by weight in the cosmetic, more preferably 2 It is good to use so that -4 weight% is contained. If the content is less than 1% by weight, sufficient whitening effect can not be obtained, and even if the content is more than 5% by weight, not only the improvement of the whitening effect can not be expected but problems such as stickiness and odor change occur. There is.
本願発明に用いられる（Ｂ）疎水化処理シリカ被覆酸化チタンは、酸化チタン粒子の平均一次粒子径が０．１μｍ以下のものを使用することが好ましい。酸化チタン粒子の粒子径が０．１μｍを超えると、隠蔽力が大きく、白くなり、透明性が低い。酸化チタン粒子の平均一次粒子径の下限は、特に限定されるものではないが、通常、０．０１μｍである。本願発明において、酸化チタン粒子の平均一次粒子径は、レーザー回折・散乱法により粒度分布を測定することで求められる。 As the (B) hydrophobized silica-coated titanium oxide used in the present invention, it is preferable to use one having an average primary particle diameter of titanium oxide particles of 0.1 μm or less. When the particle size of the titanium oxide particles exceeds 0.1 μm, the hiding power is large, whitening and transparency are low. The lower limit of the average primary particle size of the titanium oxide particles is not particularly limited, but is usually 0.01 μm. In the present invention, the average primary particle size of the titanium oxide particles can be determined by measuring the particle size distribution by a laser diffraction / scattering method.
酸化チタンに被覆するシリカは、結晶性でも非結晶性でもよい。シリカ被覆方法としては特に限定されず、公知の方法にて処理することができる（特許文献５）。例えば、酸化チタン水性懸濁液にシリカゾルを添加して、シリカを酸化チタン表面に析出させる方法などが挙げられる。 The silica coated on titanium oxide may be crystalline or non-crystalline. It does not specifically limit as a silica coating method, It can process by a well-known method (patent document 5). For example, there is a method of adding silica sol to an aqueous suspension of titanium oxide to precipitate silica on the surface of titanium oxide.
（Ｂ）疎水化処理シリカ被覆酸化チタン中のシリカ含有量は、３０重量％以上であることが好ましい。３０重量％以上であれば、アスコルビン酸−２−リン酸塩を安定に含有した化粧料を得ることができる。 (B) The silica content in the hydrophobized silica-coated titanium oxide is preferably 30% by weight or more. If it is 30 weight% or more, cosmetics which contained ascorbic acid 2-phosphate stably can be obtained.
シリカ被覆酸化チタンは、市販品を用いることもできる。例えば「マックスライトＴＳ−０１」、「マックスライトＴＳ−０４」（昭和電工株式会社製）等を挙げることができ、これらを疎水化処理して好適に用いることができる。 A commercially available product can also be used as the silica-coated titanium oxide. For example, “Max Light TS-01”, “Max Light TS-04” (manufactured by Showa Denko KK), etc. can be mentioned, and these can be suitably used after being subjected to hydrophobic treatment.
疎水化処理の方法としては、特に限定されるものでなく、公知の方法にて処理することができる。例えばメチルハイドロジェンポリシロキサン、メチルハイドロジェンポリシロキサン・ジメチルポリシロキサンコポリマー、ジメチルポリシロキサン等のシリコーン類を用いた処理；オクチルトリエトキシシラン、ヘキシルトリメトキシシラン等のシラン化合物を用いた処理；パルミチン酸、ステアリン酸等の脂肪酸を用いた処理；パーフルオロアルキルトリメトキシシラン等を用いたフッ素処理等が挙げられる。 It does not specifically limit as a method of a hydrophobization process, It can process by a well-known method. For example, treatment with silicones such as methylhydrogenpolysiloxane, methylhydrogenpolysiloxane / dimethylpolysiloxane copolymer, dimethylpolysiloxane, etc. Treatment with a silane compound such as octyltriethoxysilane, hexyltrimethoxysilane, etc .; palmitic acid And treatments with fatty acids such as stearic acid; and fluorine treatments with perfluoroalkyltrimethoxysilane and the like.
（Ｂ）疎水化処理シリカ被覆酸化チタン中の疎水化処理剤の含有量は、５重量％以上であることが好ましい。疎水化処理剤が５重量％を下回ると疎水性が不十分になり、水相のアスコルビン酸−２−リン酸塩と直接的に相互作用してしまう結果、アスコルビン酸−２−リン酸塩の安定性が著しく低下してしまう。 The content of the hydrophobizing agent in the hydrophobized silica-coated titanium oxide (B) is preferably 5% by weight or more. When the hydrophobizing agent is less than 5% by weight, the hydrophobicity becomes insufficient and directly interacts with ascorbic acid-2-phosphate in the aqueous phase, resulting in the formation of ascorbic acid-2-phosphate. The stability is significantly reduced.
なお、（Ｂ）疎水化処理シリカ被覆酸化チタン中の酸化チタン量及びシリカ被覆量は、医薬部外品原料規格２００６記載の「微粒子酸化チタン」及び「無水ケイ酸」の定量法に準じた。 The amount of titanium oxide and the amount of silica coating in (B) hydrophobized silica-coated titanium oxide were according to the quantitative method of “fine particle titanium oxide” and “anhydrous silicic acid” described in the quasi-drug raw material standard 2006.
（Ｂ）疎水化処理シリカ被覆酸化チタンの含有量は、特に限定されないが、酸化チタン純分として化粧料中３〜６重量％含有することが好ましく、４〜５重量％含有することがより好ましい。酸化チタン純分として含有量が３重量％未満であると十分な紫外線防御効果が得られず、また、６重量％を越えて含有するときしみ感などの使用感の悪化やアスコルビン酸−２−リン酸塩の安定性の低下が生じることがある。 The content of the hydrophobized silica-coated titanium oxide (B) is not particularly limited, but is preferably 3 to 6% by weight, more preferably 4 to 5% by weight, in the cosmetic as a pure titanium oxide component. . If the content is less than 3% by weight as pure titanium oxide, a sufficient ultraviolet light protective effect can not be obtained, and when it is contained in more than 6% by weight, deterioration of feeling in use such as stain and ascorbic acid-2-phosphorus A decrease in the stability of the acid salt may occur.
（Ｂ）疎水化処理シリカ被覆酸化チタンは、市販品を用いることもできる。例えば、「ＳＩ−マックスライトＴＳ−０１」、「ＳＩ−マックスライトＴＳ−０４」（三好化成工業株式会社製）等が挙げられる。 A commercial item can also be used for (B) hydrophobization process silica-coated titanium oxide. For example, "SI-Max Light TS-01", "SI-Max Light TS-04" (manufactured by Miyoshi Kasei Kogyo Co., Ltd.), etc. may be mentioned.
また、酸化チタンの代わりに酸化亜鉛を用いてシリカ被覆処理及び疎水化処理を行った。得られた疎水化処理シリカ被覆酸化亜鉛を含有した油中水型乳化化粧料を調製し、アスコルビン酸−２−リン酸塩の安定性評価を行ったが、経時的に残存率が低下してしまった。これは、酸化亜鉛に本願発明のシリカ被覆処理及び疎水化処理を用いても、亜鉛イオンの水相中への溶出が抑えられず、亜鉛イオンがアスコルビン酸−２−リン酸塩と直接的に相互作用してしまったためだと考えられる。 In addition, silica coating treatment and hydrophobization treatment were performed using zinc oxide instead of titanium oxide. The obtained water-in-oil type emulsified cosmetic containing hydrophobized silica-coated zinc oxide was prepared, and the stability of ascorbic acid-2-phosphate was evaluated, but the residual rate decreased with time. Oops. This means that even if zinc oxide is treated with the silica coating treatment and hydrophobization treatment of the present invention, elution of zinc ion into the aqueous phase can not be suppressed, and zinc ion directly with ascorbic acid-2-phosphate It is thought that it is because it has interacted.
ハンセン溶解度パラメーターδは、ヒルデブランドによって導入された溶解度パラメーターを、分散項δｄ、極性項δｐ、水素結合項δｈの３成分に分割し、３次元空間に表したものである。分散項δｄは無極性相互作用、極性項δｐは双極子間力、水素結合項δｈは水素結合力を示す。本願発明において、油剤のハンセン溶解度パラメーターδは、油剤の化学構造に基づいて算出することができる。具体的には、次式（１）を用いて計算することができる。
δ＝（δｄ２＋δｐ２＋δｈ２）０．５・・・（１）
δ：ハンセン溶解度パラメーター
δｄ：分散項
δｐ：極性項
δｈ：水素結合項
式（１）中、分散項δｄ、極性項δｐ、水素結合項δｈは、下記のように原子団のモル引力定数（Ｆｄｉ、Ｆｐｉ、Ｅｈｉ）に基づいて次式（２）〜（４）を用いて計算できる。モル引力定数に関しては、Ｋｒｅｖｅｌｅｎらにより定められた値を用い（非特許文献５）、モル体積（Ｖｉ）に関してはＦｅｄｏｒｓにより定められた原子団の体積値を用いた（非特許文献６）。
δｄ＝ΣＦｄｉ／ΣＶｉ・・・・・・・・・・・（２）
δｐ＝（ΣＦｐｉ２）０．５／ΣＶｉ・・・・・・・（３）
δｈ＝（ΣＥｈｉ／ΣＶｉ）０．５・・・・・・・（４）
Ｆｄｉ、Ｆｐｉ、Ｅｈｉ：モル引力定数、Ｖｉ：モル体積
The Hansen solubility parameter δ is obtained by dividing the solubility parameter introduced by Hildebrand into three components, a dispersion term δd, a polar term δp, and a hydrogen bond term δh, in a three-dimensional space. The dispersion term δd is a nonpolar interaction, the polar term δp is an interdipolar force, and the hydrogen bonding term δh is a hydrogen bonding force. In the present invention, the Hansen solubility parameter δ of the oil can be calculated based on the chemical structure of the oil. Specifically, it can be calculated using the following equation (1).
δ = (δd 2 + δp 2 + δh 2 ) 0.5 (1)
δ: Hansen solubility parameter δd: Dispersion term δp: Polar term δh: Hydrogen bonding term In the formula (1), the dispersion term δd, the polar term δp, and the hydrogen bonding term δh are the molar attractive constants (Fdi of atomic groups as described below) , Fpi, Ehi) and can be calculated using the following equations (2) to (4). As for the molar attraction constant, the value determined by Krevelen et al. (Non-patent Document 5) was used, and for the molar volume (Vi), the volume value of the group defined by Fedors was used (Non-patent document 6).
δ d = F F di / ・ Vi (2)
δp = (ΣFpi 2 ) 0.5 / ΣVi (3)
δh = (ΣEhi / ΣVi) 0.5 ········ (4)
Fdi, Fpi, Ehi: molar attraction constant, Vi: molar volume
本願発明に用いられる（Ｃ）ハンセン溶解度パラメーターδが１７〜２１ＭＰａ０．５の範囲にある油剤は、通常化粧料に用いられるものであれば特に限定されない。具体的には、ラウロイルサルコシンイソプロピル（δ＝２０．６、原料名：エルデュウ ＳＬ−２０５、味の素株式会社製）、安息香酸フェネチル（δ＝１９．４、原料名：Ｘ−ＴＥＮＤ ２２６、Ａｓｈｌａｎｄ ＩＮＣ製）、トリイソノナノイン（δ＝１７．１、原料名：ＩＳＯＤＲＡＧＯＬ、シムライズ株式会社製）等が挙げられ、これらの１種又は２種以上を用いることができる。 The oil agent having a Hansen solubility parameter δ in the range of 17 to 21 MPa 0.5 , which is used in the present invention, is not particularly limited as long as it is generally used for cosmetics. Specifically, lauroyl sarcosine isopropyl (.delta. = 20.6, raw material name: ELDUU SL-205, manufactured by Ajinomoto Co., Ltd.), phenethyl benzoate (.delta. = 19.4, raw material name: X-TEND 226, manufactured by Ashland INC. And triisononanoin (.delta. = 17.1, raw material name: ISODRAGOL, manufactured by Shimlize Co., Ltd.), etc., and one or more of these may be used.
（Ｃ）ハンセン溶解度パラメーターδが１７〜２１ＭＰａ０．５の範囲にある油剤の含有量は、特に限定されないが、５〜１５重量％が好ましく、７〜１２重量％がより好ましい。５重量％より少ない場合には、（Ｂ）疎水化処理シリカ被覆酸化チタンの分散性を高める効果が期待できない場合があり、１５重量％よりも多い場合には、べたつくなど使用感が悪くなる場合がある。 (C) The content of the oil agent having a Hansen solubility parameter δ in the range of 17 to 21 MPa 0.5 is not particularly limited, but 5 to 15% by weight is preferable, and 7 to 12% by weight is more preferable. If the amount is less than 5% by weight, the effect of enhancing the dispersibility of the (B) hydrophobized silica-coated titanium oxide may not be expected, and if it is more than 15% by weight, the feeling of use such as stickiness may deteriorate. There is.
本願発明の油中水型乳化化粧料は、本願発明の効果を損なわない範囲で必要に応じて、前記成分以外の各種成分、例えば、紫外線吸収剤、ｐＨ調整剤、油剤、保湿剤、水性成分、界面活性剤、酸化防止剤、美容成分、防腐剤、水溶性高分子、皮膜形成剤、褪色防止剤、消泡剤、香料等を各種の効果を付与するために適宜含有することができる。特に、紫外線吸収剤を組み合わせることによって、広いＵＶ領域で高い紫外線防御効果を発揮する。特にＵＶＡ領域の紫外線吸収剤とＵＶＢ領域の紫外線吸収剤を組み合わせることによって広いＵＶ領域で高い紫外線防御効果を発揮する。 The water-in-oil type emulsified cosmetic of the present invention may contain various components other than the above components, for example, UV absorbers, pH adjusters, oil agents, moisturizers, aqueous components, as needed, as long as the effects of the present invention are not impaired. Surfactants, antioxidants, cosmetic ingredients, preservatives, water-soluble polymers, film-forming agents, anti-fading agents, antifoaming agents, perfumes and the like can be suitably contained to impart various effects. In particular, the combination of UV absorbers exerts a high UV protection effect in a wide UV range. In particular, by combining the UV absorber in the UVA region and the UV absorber in the UVB region, a high UV protective effect is exhibited in a wide UV region.
以下に実施例を挙げて、本願発明を更に詳細に説明する。尚、これらは本願発明を何ら限定するものではない。含有量は重量％である。 The present invention will be described in more detail by way of the following examples. In addition, these do not limit the present invention at all. The content is% by weight.
実施例に先立ち、本願発明で用いた効果試験方法について述べる。 Prior to the examples, an effect test method used in the present invention will be described.
［加速試験による安定性］
（１）乳化粒子の経時安定性
化粧料を温度４０℃、相対湿度７５％の条件で３ヶ月間保存した。乳化粒子を顕微鏡にて観察し、下記の基準に従って判定した。
（評価基準）
◎：乳化粒子の粒径は初期状態と差異が認められない
○：乳化粒子の粒径が明らかに大きくなっているが乳化状態を保っている
×：結晶析出・乳化粒子が崩壊している
[Stability by accelerated test]
(1) Temporal stability of emulsified particles The cosmetic was stored for 3 months at a temperature of 40 ° C. and a relative humidity of 75%. The emulsified particles were observed with a microscope and judged according to the following criteria.
(Evaluation criteria)
:: No difference in the particle diameter of the emulsified particles from the initial state is recognized ○: The particle diameter of the emulsified particles is clearly increased but the emulsified state is maintained. ×: Crystal precipitation, the emulsified particles are disintegrated
（２）分散状態の経時安定性
化粧料を温度４０℃、相対湿度７５％の条件で３ヶ月間保存した。顕微鏡及び目視にて観察し、下記の基準に従って判定した。
（評価基準）
◎：均一に分散しており、初期状態とほとんど差異が認められない
○：凝集がやや進行しているが、目視では判別できない
×：凝集が進行し、ゲル化等が目視でも確認できる
(2) Stability over time of dispersed state The cosmetic was stored for 3 months under the conditions of temperature 40 ° C. and relative humidity 75%. It observed by the microscope and visual observation, and determined according to the following reference | standard.
(Evaluation criteria)
:: uniformly dispersed, almost no difference from the initial state is recognized ○: aggregation is slightly progressing but can not be determined visually: x: aggregation is progressing, gelation etc can be confirmed visually
（３）アスコルビン酸−２−リン酸マグネシウム安定性の評価
化粧料を温度４０℃、相対湿度７５％の条件で３ヶ月間保存した。高速液体クロマトグラフィーを用いて化粧料中のアスコルビン酸−２−リン酸マグネシウムの定量分析を行い下記基準で評価した。なお、定量法は、医薬部外品原料規格２００６に記載の「リン酸Ｌ−アスコルビルマグネシウム」の定量法に準じた。そして、定量したアスコルビン酸−２−リン酸マグネシウムの含有量を、保存開始時における同化合物の含有量を１００％としたときの相対値（％：残存率）として評価した。
◎：アスコルビン酸−２−リン酸マグネシウム残存率が９５％以上
○：アスコルビン酸−２−リン酸マグネシウム残存率が９０％以上９５％未満
×：アスコルビン酸−２−リン酸マグネシウム残存率が９０％未満
(3) Evaluation of Ascorbic Acid 2-Phosphate Magnesium Stability The cosmetic was stored for 3 months at a temperature of 40 ° C. and a relative humidity of 75%. Quantitative analysis of magnesium ascorbyl 2-phosphate in cosmetics was conducted using high performance liquid chromatography, and evaluated according to the following criteria. In addition, the quantitative method followed the quantitative method of "L-ascorbyl magnesium phosphate" described in the quasi-drug raw material standard 2006. Then, the content of the quantified ascorbic acid-2-phosphate magnesium was evaluated as a relative value (%: residual rate) when the content of the same compound at the start of storage was 100%.
:: 95% or more of the ascorbic acid-2-phosphate residual ratio :: 90% to less than 95% of the ascorbic acid 2-phosphate residual ratio ×: 90% of the ascorbic acid 2-phosphate residual ratio Less than
［使用感］
（１）べたつきのなさ
専門パネル２０名により、各化粧料について、肌に塗布した際のべたつきのなさについて使用テストを行い、アンケートの結果から下記の基準に従って判定した。
（評価基準）
◎：２０名中、１５名以上がべたつかないと回答した
○：２０名中、１０〜１４名がべたつかないと回答した
△：２０名中、５〜９名がべたつかないと回答した
×：２０名中、４名以下がべたつかないと回答した
[Feeling of use]
(1) Lack of Stickiness The use test was carried out by each of the professional panels with respect to each cosmetic with respect to no tackiness when applied to the skin by 20 persons, and it was judged according to the following criteria from the result of the questionnaire.
(Evaluation criteria)
:: 20 or more answered that 15 or more were not sticky ○: out of 20 10 to 14 answered that it was not sticky 20: 5 to 20 out of 20 people answered that was not sticky ×: 20 In the name, four or less answered that they were not sticky
（２）きしみ感のなさ
専門パネル２０名により、各化粧料について、肌に塗布した際のきしみ感のなさについて使用テストを行ない、アンケートの結果から下記の基準に従って判定した。
（評価基準）
◎：２０名中、１５名以上がきしまないと回答した
○：２０名中、１０〜１４名がきしまないと回答した
△：２０名中、５〜９名がきしまないと回答した
×：２０名中、４名以下がきしまないと回答した
(2) Lack of squeakiness The use test was carried out by each of the professional panels with 20 people for the squeakiness of each cosmetic when applied to the skin, and it was judged from the result of the questionnaire according to the following criteria.
(Evaluation criteria)
:: 20 out of 20 people answered that no more than 15 people ○: out of 20 people answered that 10 to 14 people out of △: 5 out of 20 people said that 5 to 9 people did not respond ×: 20 In the name, I replied that 4 people or less would not come
表１及び表２に示す処方の油中水型乳化化粧料を調製し、乳化粒子の経時安定性、分散安定性、アスコルビン酸−２−リン酸マグネシウム安定性、使用感の評価を前記の基準に従って行った。 Preparation of water-in-oil type emulsion cosmetic of the formulation shown in Table 1 and Table 2, the above-mentioned criteria of evaluation of stability over time of emulsion particles, dispersion stability, magnesium ascorbic acid 2-phosphate stability, feeling of use. It went according to.
表１及び表２の処方により得られた油中水型乳化化粧料は、以下に示す製造方法により調製した。
（製造方法）
油相、水相をそれぞれ均一に分散した。油相へ水相を撹拌しながら徐々に添加して、常温にてホモミキサーを５０００ｒｐｍで５分間運転することで乳化した。乳化後、脱泡して表１及び表２の油中水型乳化化粧料を得た。
The water-in-oil type emulsified cosmetic obtained by the formulations of Table 1 and Table 2 was prepared by the production method shown below.
(Production method)
The oil phase and the aqueous phase were each dispersed uniformly. The aqueous phase was gradually added to the oil phase while stirring, and emulsification was performed by operating a homomixer at 5000 rpm for 5 minutes at normal temperature. After emulsification, the mixture was defoamed to obtain a water-in-oil emulsified cosmetic of Table 1 and Table 2.
表１に示す結果から、（Ａ）アスコルビン酸−２−リン酸塩及び３０重量％以上のシリカ被覆量であり５重量％以上の疎水化処理剤含有量である（Ｂ）疎水化処理シリカ被覆酸化チタンを含有する化粧料（実施例１〜９）は、優れた使用感を有し、（Ａ）アスコルビン酸−２−リン酸塩安定性及び化粧料の安定性も優れていることが分かる。一方、酸化チタンのシリカ処理が３０重量％に満たない場合、又は疎水化処理が５重量％に満たない化粧料（比較例１〜７）では、満足な使用感又は（Ａ）アスコルビン酸−２−リン酸塩及び／又は化粧料の安定性が得られなかった。 From the results shown in Table 1, (A) Ascorbic acid-2-phosphate and silica coating amount of 30% by weight or more, and 5% by weight or more of hydrophobizing agent content (B) Hydrophobicized silica coating Cosmetics containing titanium oxide (Examples 1 to 9) have excellent feeling in use, and it can be seen that (A) ascorbic acid-2-phosphate stability and cosmetic stability are also excellent. . On the other hand, when the silica treatment of titanium oxide is less than 30% by weight, or in the cosmetic wherein the hydrophobization treatment is less than 5% by weight (comparative examples 1 to 7), the feeling of use satisfactory or (A) ascorbic acid-2 -No stability of phosphate and / or cosmetic was obtained.
表２に示す結果から、（Ａ）アスコルビン酸−２−リン酸塩及び３０重量％以上のシリカ被覆量であり５重量％以上の疎水化処理剤含有量である（Ｂ）疎水化処理シリカ被覆酸化チタンを含有する化粧料（実施例１０〜１８）は、優れた使用感を有し、（Ａ）アスコルビン酸−２−リン酸塩の安定性及び化粧料の安定性も優れており、本願発明効果が得られた。特に、（Ｃ）ハンセン溶解度パラメーターδが１７〜２１ＭＰａ０．５の油剤を含有する油中水型乳化化粧料（実施例１０〜１５）は、すべての評価項目において格段に優れた評価結果であった。 From the results shown in Table 2, (A) Ascorbic acid-2-phosphate and silica coating amount of 30% by weight or more, and 5% by weight or more of hydrophobizing agent content (B) Hydrophobicized silica coating Cosmetics containing titanium oxide (Examples 10 to 18) have excellent feeling in use, and (A) stability of ascorbic acid-2-phosphate and stability of cosmetics are also excellent. Invention effects were obtained. In particular, the water-in-oil type emulsified cosmetic (Examples 10 to 15) containing an oil having a Hansen solubility parameter δ of 17 to 21 MPa 0.5 (C) is an evaluation result that is extremely excellent in all evaluation items. The
なお、表１及び表２中、以下に示す成分は下記製品を用いた。
※１ ＳＩ−マックスライト ＴＳ−０４ （三好化成工業株式会社製）
※２ ＳＩ−マックスライト ＴＳ−０１ （三好化成工業株式会社製）
※３ ＳＴＲ−１００Ｗ−ＬＰ （堺化学工業株式会社製）
※４ マックスライト ＴＳ−０４−Ｄ （昭和電工株式会社製）
※５ マックスライト ＴＳ−０４３−Ｄ （昭和電工株式会社製）
※６ ＭＴ−０２ （テイカ株式会社製）
※７ ＭＴ−０１ （テイカ株式会社製）
※８ エルデュウ ＳＬ−２０５ （味の素株式会社製）
※９ マックスライト ＴＳ−０４ （昭和電工株式会社製）
※１０ ＳＴＲ−１００Ｗ （堺化学工業株式会社製）
※１１ セバチン酸ジエチル （日本精化株式会社製）
※１２ クロダモル ＯＳＵ （クローダジャパン株式会社製）
※１３ ＥＩＳ−Ｖ （高級アルコール工業株式会社製）
※１４ ＮＰＤＩＮ （高級アルコール工業株式会社製）
※１５ Ｅｌｅｆａｃ Ｉ−２０５（Ｂｅｒｎｅｌ Ｃｈｅｍｉｃａｌ Ｃｏｍｐａｎｙ製）
In Tables 1 and 2, the following products were used as the components shown below.
* 1 SI-Max Light TS-04 (made by Miyoshi Kasei Kogyo Co., Ltd.)
* 2 SI-Max Light TS-01 (made by Miyoshi Kasei Kogyo Co., Ltd.)
* 3 STR-100W-LP (made by Sakai Chemical Industry Co., Ltd.)
* 4 Maxlight TS-04-D (manufactured by Showa Denko KK)
* 5 Max Light TS-043-D (manufactured by Showa Denko KK)
※ 6 MT-02 (made by Tayca Corporation)
※ 7 MT-01 (made by Tayca Corporation)
* 8 ELDU SL-205 (made by Ajinomoto Co., Ltd.)
* 9 Maxlight TS-04 (manufactured by Showa Denko KK)
※ 10 STR-100W (made by Sakai Chemical Industry Co., Ltd.)
* 11 Diethyl sebacate (manufactured by Nippon Seika Co., Ltd.)
* 12 Kurodamol OSU (made by Croda Japan KK)
※ 13 EIS-V (made by luxury alcohol industry Ltd.)
※ 14 NPDIN (made by high-grade alcohol industry Ltd.)
* 15 Elefac I-205 (manufactured by Bernel Chemical Company)
以下に本願発明を、詳細に説明するため実施例を挙げて説明する。 Hereinafter, the present invention will be described by way of examples in order to explain the present invention in detail.
実施例１９ クリーム状美白日焼け止め化粧料
含有成分 含有量（重量％）
油相
（１） ジエチルアミノヒドロキシベンゾイル安息香酸ヘキシル ２．００
（２） メトキシケイヒ酸エチルヘキシル １０．００
（３） ラウロイルサルコシンイソプロピル※８ １２．００
（４） デカメチルテトラシロキサン １２．００
（５） ネオペンタン酸オクチルドデシル※１５ １０．００
（６） ペンタオキシステアリン酸デカグリセリル １．００
（７） ジポリヒドロキシステアリン酸ＰＥＧ−３０ ０．５０
（８） ５％シリコーン処理３１％シリカ被覆酸化チタン※１ ５．００
（９） ジステアルジモニウムヘクトライト １．５０
水相
（１０） 精製水 残量
（１１） １，３−ブチレングリコール １０．００
（１２） アスコルビン酸−２−リン酸ナトリウム ３．００
（１３） クエン酸ナトリウム ３．００
（１４） ＥＤＴＡ−４Ｎａ ０．１０
（１５） エタノール ４．００
（１６） パラオキシ安息香酸メチル ０．２０
Example 19: Creamy whitening sunscreen composition content (% by weight)
Oil phase (1) Diethylamino hydroxybenzoyl hexyl 2.00
(2) Ethylhexyl methoxycinnamate 10.00
(3) lauroyl sarcosine isopropyl * 8 12.00
(4) Decamethyltetrasiloxane 12.00
(5) Octopyl dodecyl neopentanoate * 15 10.00
(6) Decaglyceryl pentaoxystearate 1.00
(7) Dipolyhydroxystearic acid PEG-30 0.50
(8) 5% silicone treatment 31% silica coated titanium oxide * 1 5.00
(9) distardimonium hectorite 1.50
Water phase (10) Purified water balance (11) 1,3-butylene glycol 10.00
(12) Ascorbic acid-2-phosphate sodium 3.00
(13) Sodium citrate 3.00
(14) EDTA-4Na 0.10
(15) Ethanol 4.00
(16) Methyl parahydroxybenzoate 0.20
（調製方法）
成分（１）を成分（２）に加熱溶解後、成分（３）〜（９）を加えて均一に分散した。これに成分（１０）〜（１６）の混合水溶液を加え、常温にてホモミキサーを５０００ｒｐｍで５分間運転することで乳化した。乳化後、脱泡して油中水型乳化化粧料を得た。
(Preparation method)
After heat-dissolving component (1) to component (2), components (3) to (9) were added and dispersed uniformly. The mixed aqueous solution of component (10)-(16) was added to this, and it emulsified by operating a homomixer at 5000 rpm for 5 minutes at normal temperature. After emulsification, the mixture was defoamed to obtain a water-in-oil emulsified cosmetic.
（Ａ）アスコルビン酸−２−リン酸塩及び（Ｂ）疎水化処理シリカ被覆酸化チタンを含有した実施例１９は、優れた使用感を有し、（Ａ）アスコルビン酸−２−リン酸塩の安定性及び化粧料の安定性も優れていた。美白効果と紫外線防御効果を併せ持ち、経時的に安定性の高い油中水型乳化化粧料が得られた。 Example 19 containing (A) ascorbic acid 2-phosphate and (B) hydrophobized silica-coated titanium oxide has excellent feeling of use, and (A) ascorbic acid 2-phosphate The stability and the stability of the cosmetic were also excellent. A water-in-oil type emulsified cosmetic having high whitening effect and ultraviolet light protective effect and high stability over time was obtained.
本願発明によれば、美白効果と紫外線防御効果を両立し、かつ経時的に安定性の高い油中水型乳化化粧料を提供できる。
According to the present invention, it is possible to provide a water-in-oil type emulsified cosmetic which achieves both the whitening effect and the ultraviolet light protective effect and has high stability over time.
Claims (1)
（Ａ）化１で表わされるアスコルビン酸−２−リン酸塩 １重量％〜５重量％
（Ｃ）ハンセン溶解度パラメーターδが１７〜２１ＭＰａ ０．５ の油剤 ５重量％〜１５重量％
を含有し、（Ｂ）疎水化処理シリカ被覆酸化チタン中、シリカ被覆量が３０重量％以上であり、疎水化処理剤の含有量が５重量％以上であることを特徴とする油中水型乳化化粧料。 The following components (A) , (B) and (C) ;
(A) 1 wt% to 5 wt% of ascorbic acid-2-phosphate represented by Chemical Formula 1
(C) Hansen solubility parameter δ: 17 to 21 MPa 0.5 oil agent 5 wt% to 15 wt%
Water-in-oil type characterized in that the coating amount of silica in the (B) hydrophobized treated silica-coated titanium oxide is at least 30% by weight and the content of the hydrophobizing agent is at least 5% by weight. Emulsion cosmetic.
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