CN117017831B - 一种美白抗初老洁面乳及其制备工艺 - Google Patents
一种美白抗初老洁面乳及其制备工艺 Download PDFInfo
- Publication number
- CN117017831B CN117017831B CN202311158058.4A CN202311158058A CN117017831B CN 117017831 B CN117017831 B CN 117017831B CN 202311158058 A CN202311158058 A CN 202311158058A CN 117017831 B CN117017831 B CN 117017831B
- Authority
- CN
- China
- Prior art keywords
- parts
- whitening
- facial cleanser
- acid
- component
- 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
- 230000001815 facial effect Effects 0.000 title claims abstract description 44
- 230000002087 whitening effect Effects 0.000 title claims abstract description 36
- 230000003712 anti-aging effect Effects 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 9
- POJWUDADGALRAB-UHFFFAOYSA-N allantoin Chemical compound NC(=O)NC1NC(=O)NC1=O POJWUDADGALRAB-UHFFFAOYSA-N 0.000 claims abstract description 32
- 108090000765 processed proteins & peptides Proteins 0.000 claims abstract description 25
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 229920002770 condensed tannin Polymers 0.000 claims abstract description 18
- 235000018192 pine bark supplement Nutrition 0.000 claims abstract description 18
- 229940106796 pycnogenol Drugs 0.000 claims abstract description 18
- KSEBMYQBYZTDHS-HWKANZROSA-M (E)-Ferulic acid Natural products COC1=CC(\C=C\C([O-])=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-M 0.000 claims abstract description 16
- RFWGABANNQMHMZ-UHFFFAOYSA-N 8-acetoxy-7-acetyl-6,7,7a,8-tetrahydro-5H-benzo[g][1,3]dioxolo[4',5':4,5]benzo[1,2,3-de]quinoline Natural products CC=C1C(CC(=O)OCCC=2C=C(O)C(O)=CC=2)C(C(=O)OC)=COC1OC1OC(CO)C(O)C(O)C1O RFWGABANNQMHMZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- POJWUDADGALRAB-PVQJCKRUSA-N Allantoin Natural products NC(=O)N[C@@H]1NC(=O)NC1=O POJWUDADGALRAB-PVQJCKRUSA-N 0.000 claims abstract description 16
- 240000005343 Azadirachta indica Species 0.000 claims abstract description 16
- 229920001661 Chitosan Polymers 0.000 claims abstract description 16
- AERBNCYCJBRYDG-UHFFFAOYSA-N D-ribo-phytosphingosine Natural products CCCCCCCCCCCCCCC(O)C(O)C(N)CO AERBNCYCJBRYDG-UHFFFAOYSA-N 0.000 claims abstract description 16
- HKVGJQVJNQRJPO-UHFFFAOYSA-N Demethyloleuropein Natural products O1C=C(C(O)=O)C(CC(=O)OCCC=2C=C(O)C(O)=CC=2)C(=CC)C1OC1OC(CO)C(O)C(O)C1O HKVGJQVJNQRJPO-UHFFFAOYSA-N 0.000 claims abstract description 16
- BIVBRWYINDPWKA-VLQRKCJKSA-L Glycyrrhizinate dipotassium Chemical compound [K+].[K+].O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@H]1CC[C@]2(C)[C@H]3C(=O)C=C4[C@@H]5C[C@](C)(CC[C@@]5(CC[C@@]4(C)[C@]3(C)CC[C@H]2C1(C)C)C)C(O)=O)C([O-])=O)[C@@H]1O[C@H](C([O-])=O)[C@@H](O)[C@H](O)[C@H]1O BIVBRWYINDPWKA-VLQRKCJKSA-L 0.000 claims abstract description 16
- 235000013500 Melia azadirachta Nutrition 0.000 claims abstract description 16
- ATGQXSBKTQANOH-UWVGARPKSA-N N-oleoylphytosphingosine Chemical compound CCCCCCCCCCCCCC[C@@H](O)[C@@H](O)[C@H](CO)NC(=O)CCCCCCC\C=C/CCCCCCCC ATGQXSBKTQANOH-UWVGARPKSA-N 0.000 claims abstract description 16
- RFWGABANNQMHMZ-HYYSZPHDSA-N Oleuropein Chemical compound O([C@@H]1OC=C([C@H](C1=CC)CC(=O)OCCC=1C=C(O)C(O)=CC=1)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O RFWGABANNQMHMZ-HYYSZPHDSA-N 0.000 claims abstract description 16
- 229960000458 allantoin Drugs 0.000 claims abstract description 16
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims abstract description 16
- 229940101029 dipotassium glycyrrhizinate Drugs 0.000 claims abstract description 16
- KSEBMYQBYZTDHS-HWKANZROSA-N ferulic acid Chemical compound COC1=CC(\C=C\C(O)=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-N 0.000 claims abstract description 16
- 229940114124 ferulic acid Drugs 0.000 claims abstract description 16
- KSEBMYQBYZTDHS-UHFFFAOYSA-N ferulic acid Natural products COC1=CC(C=CC(O)=O)=CC=C1O KSEBMYQBYZTDHS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000001785 ferulic acid Nutrition 0.000 claims abstract description 16
- RFWGABANNQMHMZ-CARRXEGNSA-N oleuropein Natural products COC(=O)C1=CO[C@@H](O[C@H]2O[C@@H](CO)[C@H](O)[C@@H](O)[C@@H]2O)C(=CC)[C@H]1CC(=O)OCCc3ccc(O)c(O)c3 RFWGABANNQMHMZ-CARRXEGNSA-N 0.000 claims abstract description 16
- 235000011576 oleuropein Nutrition 0.000 claims abstract description 16
- 229940033329 phytosphingosine Drugs 0.000 claims abstract description 16
- 229920002643 polyglutamic acid Polymers 0.000 claims abstract description 16
- -1 salicyl phytosphingosine Chemical compound 0.000 claims abstract description 16
- QURCVMIEKCOAJU-UHFFFAOYSA-N trans-isoferulic acid Natural products COC1=CC=C(C=CC(O)=O)C=C1O QURCVMIEKCOAJU-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 14
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 claims abstract description 11
- 229940035437 1,3-propanediol Drugs 0.000 claims abstract description 11
- 229920000166 polytrimethylene carbonate Polymers 0.000 claims abstract description 11
- 239000001397 quillaja saponaria molina bark Substances 0.000 claims abstract description 3
- 229930182490 saponin Natural products 0.000 claims abstract description 3
- 150000007949 saponins Chemical class 0.000 claims abstract description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 42
- 241000243812 Arenicola marina Species 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 22
- 239000004094 surface-active agent Substances 0.000 claims description 21
- 239000003995 emulsifying agent Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 16
- 239000000344 soap Substances 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- KQEQPUBSXXOUGC-MLCQCVOFSA-N (2S)-2-[[(2S)-2-[[(2S)-1-[(2S)-1-acetylpyrrolidine-2-carbonyl]pyrrolidine-2-carbonyl]amino]-3-(4-hydroxyphenyl)propanoyl]amino]-4-methylpentanoic acid Chemical compound CC(C)C[C@H](NC(=O)[C@H](Cc1ccc(O)cc1)NC(=O)[C@@H]1CCCN1C(=O)[C@@H]1CCCN1C(C)=O)C(O)=O KQEQPUBSXXOUGC-MLCQCVOFSA-N 0.000 claims description 8
- WSGCRSMLXFHGRM-DEVHWETNSA-N (2s)-2-[[(2s)-6-amino-2-[[(2s,3r)-2-[[(2s,3r)-2-[[(2s)-6-amino-2-(hexadecanoylamino)hexanoyl]amino]-3-hydroxybutanoyl]amino]-3-hydroxybutanoyl]amino]hexanoyl]amino]-3-hydroxypropanoic acid Chemical compound CCCCCCCCCCCCCCCC(=O)N[C@@H](CCCCN)C(=O)N[C@@H]([C@@H](C)O)C(=O)N[C@@H]([C@@H](C)O)C(=O)N[C@@H](CCCCN)C(=O)N[C@@H](CO)C(O)=O WSGCRSMLXFHGRM-DEVHWETNSA-N 0.000 claims description 8
- LODWEXDBRZBADB-XEVVZDEMSA-N (2s)-6-amino-2-[[(2s)-2-[[(2s)-6-amino-2-(hexadecanoylamino)hexanoyl]amino]-3-methylbutanoyl]amino]hexanoic acid Chemical group CCCCCCCCCCCCCCCC(=O)N[C@@H](CCCCN)C(=O)N[C@@H](C(C)C)C(=O)N[C@@H](CCCCN)C(O)=O LODWEXDBRZBADB-XEVVZDEMSA-N 0.000 claims description 8
- 241000195474 Sargassum Species 0.000 claims description 8
- 229940094912 palmitoyl tripeptide-5 Drugs 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 7
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 6
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- YBRJTUFWBLSLHY-UHFFFAOYSA-N 2-[2-(2-octadecanoyloxyethoxy)ethoxy]ethyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCOCCOCCOC(=O)CCCCCCCCCCCCCCCCC YBRJTUFWBLSLHY-UHFFFAOYSA-N 0.000 claims description 5
- 230000001804 emulsifying effect Effects 0.000 claims description 5
- 238000010008 shearing Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- 239000005639 Lauric acid Substances 0.000 claims description 3
- 235000021314 Palmitic acid Nutrition 0.000 claims description 3
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- 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 claims description 2
- 229940033355 lauric acid Drugs 0.000 claims description 2
- PYIDGJJWBIBVIA-UYTYNIKBSA-N lauryl glucoside Chemical compound CCCCCCCCCCCCO[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O PYIDGJJWBIBVIA-UYTYNIKBSA-N 0.000 claims description 2
- 229940048848 lauryl glucoside Drugs 0.000 claims description 2
- 229940098695 palmitic acid Drugs 0.000 claims description 2
- 229940048109 sodium methyl cocoyl taurate Drugs 0.000 claims description 2
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 18
- 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 abstract description 14
- 230000003078 antioxidant effect Effects 0.000 abstract description 5
- 102000008186 Collagen Human genes 0.000 abstract description 3
- 108010035532 Collagen Proteins 0.000 abstract description 3
- 239000003963 antioxidant agent Substances 0.000 abstract description 3
- 229920001436 collagen Polymers 0.000 abstract description 3
- 230000012010 growth Effects 0.000 abstract description 3
- 230000035699 permeability Effects 0.000 abstract description 3
- 230000004060 metabolic process Effects 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 230000002792 vascular Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 22
- 210000003491 skin Anatomy 0.000 description 18
- 230000005764 inhibitory process Effects 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 12
- 238000002835 absorbance Methods 0.000 description 8
- 239000000523 sample Substances 0.000 description 8
- 230000002401 inhibitory effect Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 230000003064 anti-oxidating effect Effects 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 6
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 6
- 102000016387 Pancreatic elastase Human genes 0.000 description 5
- 108010067372 Pancreatic elastase Proteins 0.000 description 5
- 239000000872 buffer Substances 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 102000004400 Aminopeptidases Human genes 0.000 description 4
- 108090000915 Aminopeptidases Proteins 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- 230000036564 melanin content Effects 0.000 description 4
- 210000002752 melanocyte Anatomy 0.000 description 4
- 230000009759 skin aging Effects 0.000 description 4
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical group NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 3
- 102000016942 Elastin Human genes 0.000 description 3
- 108010014258 Elastin Proteins 0.000 description 3
- 102100027998 Macrophage metalloelastase Human genes 0.000 description 3
- 101710187853 Macrophage metalloelastase Proteins 0.000 description 3
- 102000000380 Matrix Metalloproteinase 1 Human genes 0.000 description 3
- 108010016113 Matrix Metalloproteinase 1 Proteins 0.000 description 3
- 235000021360 Myristic acid Nutrition 0.000 description 3
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229920002549 elastin Polymers 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- NTYJJOPFIAHURM-UHFFFAOYSA-N Histamine Chemical compound NCCC1=CN=CN1 NTYJJOPFIAHURM-UHFFFAOYSA-N 0.000 description 2
- 102400000740 Melanocyte-stimulating hormone alpha Human genes 0.000 description 2
- 101710200814 Melanotropin alpha Proteins 0.000 description 2
- 102000005741 Metalloproteases Human genes 0.000 description 2
- 108010006035 Metalloproteases Proteins 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 102000003425 Tyrosinase Human genes 0.000 description 2
- 108060008724 Tyrosinase Proteins 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000004856 capillary permeability Effects 0.000 description 2
- 230000010261 cell growth Effects 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000007794 irritation Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 235000013336 milk Nutrition 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- 239000013642 negative control Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000008055 phosphate buffer solution Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000035755 proliferation Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- WHNFPRLDDSXQCL-UAZQEYIDSA-N α-msh Chemical compound C([C@@H](C(=O)N[C@@H](CO)C(=O)N[C@@H](CCSC)C(=O)N[C@@H](CCC(O)=O)C(=O)N[C@@H](CC=1NC=NC=1)C(=O)N[C@@H](CC=1C=CC=CC=1)C(=O)N[C@@H](CCCNC(N)=N)C(=O)N[C@@H](CC=1C2=CC=CC=C2NC=1)C(=O)NCC(=O)N[C@@H](CCCCN)C(=O)N1[C@@H](CCC1)C(=O)N[C@@H](C(C)C)C(N)=O)NC(=O)[C@H](CO)NC(C)=O)C1=CC=C(O)C=C1 WHNFPRLDDSXQCL-UAZQEYIDSA-N 0.000 description 2
- WMBWREPUVVBILR-WIYYLYMNSA-N (-)-Epigallocatechin-3-o-gallate Chemical compound O([C@@H]1CC2=C(O)C=C(C=C2O[C@@H]1C=1C=C(O)C(O)=C(O)C=1)O)C(=O)C1=CC(O)=C(O)C(O)=C1 WMBWREPUVVBILR-WIYYLYMNSA-N 0.000 description 1
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 1
- 108700023418 Amidases Proteins 0.000 description 1
- 241001127714 Amomum Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- UDMBCSSLTHHNCD-UHFFFAOYSA-N Coenzym Q(11) Natural products C1=NC=2C(N)=NC=NC=2N1C1OC(COP(O)(O)=O)C(O)C1O UDMBCSSLTHHNCD-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000010834 Extracellular Matrix Proteins Human genes 0.000 description 1
- 108010037362 Extracellular Matrix Proteins Proteins 0.000 description 1
- WMBWREPUVVBILR-UHFFFAOYSA-N GCG Natural products C=1C(O)=C(O)C(O)=CC=1C1OC2=CC(O)=CC(O)=C2CC1OC(=O)C1=CC(O)=C(O)C(O)=C1 WMBWREPUVVBILR-UHFFFAOYSA-N 0.000 description 1
- MVORZMQFXBLMHM-QWRGUYRKSA-N Gly-His-Lys Chemical compound NCCCC[C@@H](C(O)=O)NC(=O)[C@@H](NC(=O)CN)CC1=CN=CN1 MVORZMQFXBLMHM-QWRGUYRKSA-N 0.000 description 1
- WTDRDQBEARUVNC-LURJTMIESA-N L-DOPA Chemical compound OC(=O)[C@@H](N)CC1=CC=C(O)C(O)=C1 WTDRDQBEARUVNC-LURJTMIESA-N 0.000 description 1
- WTDRDQBEARUVNC-UHFFFAOYSA-N L-Dopa Natural products OC(=O)C(N)CC1=CC=C(O)C(O)=C1 WTDRDQBEARUVNC-UHFFFAOYSA-N 0.000 description 1
- 102000002274 Matrix Metalloproteinases Human genes 0.000 description 1
- 108010000684 Matrix Metalloproteinases Proteins 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 206010051246 Photodermatosis Diseases 0.000 description 1
- 102000004022 Protein-Tyrosine Kinases Human genes 0.000 description 1
- 108090000412 Protein-Tyrosine Kinases Proteins 0.000 description 1
- 239000006180 TBST buffer Substances 0.000 description 1
- 206010043189 Telangiectasia Diseases 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 239000013504 Triton X-100 Substances 0.000 description 1
- 229920004890 Triton X-100 Polymers 0.000 description 1
- UDMBCSSLTHHNCD-KQYNXXCUSA-N adenosine 5'-monophosphate Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP(O)(O)=O)[C@@H](O)[C@H]1O UDMBCSSLTHHNCD-KQYNXXCUSA-N 0.000 description 1
- 229950006790 adenosine phosphate Drugs 0.000 description 1
- 102000005922 amidase Human genes 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005842 biochemical reaction Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004113 cell culture Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007979 citrate buffer Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 210000002744 extracellular matrix Anatomy 0.000 description 1
- 210000002950 fibroblast Anatomy 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000007760 free radical scavenging Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 150000003278 haem Chemical class 0.000 description 1
- 230000036074 healthy skin Effects 0.000 description 1
- 229960001340 histamine Drugs 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 210000002510 keratinocyte Anatomy 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000006072 paste Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000008845 photoaging Effects 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 239000013641 positive control Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 150000003180 prostaglandins Chemical class 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 210000002374 sebum Anatomy 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 208000009056 telangiectasis Diseases 0.000 description 1
- PSWFFKRAVBDQEG-YGQNSOCVSA-N thymopentin Chemical compound NC(N)=NCCC[C@H](N)C(=O)N[C@@H](CCCCN)C(=O)N[C@@H](CC(O)=O)C(=O)N[C@@H](C(C)C)C(=O)N[C@H](C(O)=O)CC1=CC=C(O)C=C1 PSWFFKRAVBDQEG-YGQNSOCVSA-N 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/88—Polyamides
-
- 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
- A61K8/345—Alcohols containing more than one hydroxy group
-
- 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
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/494—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
- A61K8/4946—Imidazoles or their condensed derivatives, e.g. benzimidazoles
-
- 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
- A61K8/60—Sugars; Derivatives thereof
- A61K8/602—Glycosides, e.g. rutin
-
- 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
- A61K8/63—Steroids; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/68—Sphingolipids, e.g. ceramides, cerebrosides, gangliosides
-
- 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
- A61K8/736—Chitin; Chitosan; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9755—Gymnosperms [Coniferophyta]
- A61K8/9767—Pinaceae [Pine family], e.g. pine or cedar
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/98—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
- A61K8/987—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/10—Washing or bathing preparations
-
- 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
- A61K2800/592—Mixtures of compounds complementing their respective functions
- A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
-
- 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
- A61K2800/74—Biological properties of particular ingredients
- A61K2800/78—Enzyme modulators, e.g. Enzyme agonists
- A61K2800/782—Enzyme inhibitors; Enzyme antagonists
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
本发明提供一种美白抗初老洁面乳及其制备工艺,包括以下重量份原料:环γ‑聚谷氨酸12‑25份、阿魏酸0.3‑1.5份、沙虫体壁溶出物3‑5份、碧萝芷15‑50份、活性肽2.6‑8.9份、N‑乙酰基‑L‑鸭皂酸2.5‑5.8份、水杨酰植物鞘胺醇0.5‑1.5份、神经酰胺NP5.2‑11.9份、橄榄苦苷1.9‑5.6份、甘草酸二钾2.5‑5.9份、羧甲基脱乙酰壳多糖3.8‑5.9份、1,3‑丙二醇3.8‑6.1份、印度楝叶提取物1.5‑2.8份、尿囊素2.6‑5.9份,其中通过美白原料、抗氧化原料、具有修复作用的原料和辅料科学配比而成,具有较好的美白效果和抗初老效果,既能抑制黑色素生长的同时,还能降低血管通透性,促进皮肤新陈代谢,增加胶原蛋白弹性蛋白的功效。
Description
技术领域
本发明涉及日用化妆品领域,特别涉及一种美白抗初老洁面乳及其制备工艺。
背景技术
洁面乳,又称洗面奶,属于面部洁肤制品。清洗皮肤时,洗面奶清洗的对象物是人体面部的皮肤分泌的皮脂、汗、剥离脱落的角质层细胞等从身体上产生的污垢,以及灰尘、各种微生物、美容化妆品残留物等来自外部的污垢。这些残留代谢产物是不稳定的,可与空气中的氧,或沉积分子反应。在暴露于阳光时或皮肤上有细菌存在,会发生各种物理化学和生物化学反应,形成一些可能伤害皮肤的刺激物质。因而,即使是健康的肌肤,皮肤清洁也是皮肤护理所必须的过程。
洁面乳可以按产品形态进行分类,分为固体(皂类)、膏霜、糊状、液状/黏稠液状、颗粒/粉末状、泡沫;按主要表面活性剂种类分类,分为皂基型洗面奶、氨基酸型洗面奶、复配型洗面奶,其中,皂基体系去污去脂能力强,但使用后皮肤缺水紧绷,清洁过度,容易损伤肌肤:表面活性剂体系相对于皂基体系较温和,去污去脂能力适中,但表面活性剂不易清洗干净,洗后残留较多,停留在皮肤表面具有一定的刺激性:氨基酸表面活性剂呈弱酸性,与皮肤表面的pH值接近,亲肤性好,洗净力适中,洗后残留少,相比于皂基体系和表面活性剂体系产品温和程度高,但同样存在使用后皮肤缺水紧绷的问题:乳化体系洁面产品使用后没有缺水紧绷的不适感,但泡沫少、去污去脂能力差;随着人们生活水平的不断提高,人们对日常使用的产品也提出了更高的要求,在洁面的同时可以既能达到美白的作用,还能起到抗氧化、抗初老的效果,从而达到复配型的洗面奶,但是市面上的复配型洁面或多或少存在刺激性强,在美白、抗氧化等功能特性后,对脸部皮肤有一定的刺激性,导致皮肤毛细血管扩张,脸部出现泛红的现象,从而致使皮肤变敏感。
发明内容
鉴于此,本发明提出一种美白抗初老洁面乳及其制备工艺,解决上述问题。
本发明的技术方案是这样实现的:一种美白抗初老洁面乳:包括以下重量份原料:环γ-聚谷氨酸12-25份、阿魏酸0.3-1.5份、沙虫体壁溶出物3-5份、碧萝芷15-50份、活性肽2.6-8.9份、N-乙酰基-L-鸭皂酸2.5-5.8份、水杨酰植物鞘胺醇0.5-1.5份、神经酰胺NP5.2-11.9份、橄榄苦苷1.9-5.6份、甘草酸二钾2.5-5.9份、羧甲基脱乙酰壳多糖3.8-5.9份、1,3-丙二醇3.8-6.1份、印度楝叶提取物1.5-2.8份、尿囊素2.6-5.9份。
进一步的,一种美白抗初老洁面乳:包括以下重量份原料:环γ-聚谷氨酸20份、阿魏酸0.9份、沙虫体壁溶出物4份、碧萝芷33份、活性肽6.2份、N-乙酰基-L-鸭皂酸3.7份、水杨酰植物鞘胺醇1.0份、神经酰胺NP8.4份、橄榄苦苷4.1份、甘草酸二钾3.8份、羧甲基脱乙酰壳多糖4.8份、1,3-丙二醇5.2份、印度楝叶提取物2.2份、尿囊素3.1份。
进一步的,所述活性肽为质量比(3.6-8.5):(1.3-2.8):(11.5-18.6)的棕榈酰三肽-5、乙酰基四肽-11、棕榈酰五肽-4。
进一步的,所述沙虫体壁溶出物是将沙虫放入质量浓度为0.1-0.2‰的柠檬酸溶液中浸泡30-50min,沙虫和柠檬酸溶液的质量体积比g/mL为3-8:15,80-100℃下微波加热8-15min,超声过滤,取液体,在40-85℃下蒸发浓缩,将浓缩液在-30~-5℃下冷冻干燥,得到,沙虫体壁溶出物。
进一步的,一种美白抗初老洁面乳,还包括表面活性剂3-9份、乳化剂2-6份、水25-49份。
进一步的,所述表面活性剂为肉豆蔻酸、月桂酸、棕榈酸、甲基椰油酰基牛磺酸钠、月桂基葡糖苷中任意一种或几种组合。
进一步的,所述乳化剂为PEG-3二硬脂酸酯、山梨醇聚醚-30四油酸酯、聚甘油-10二异硬脂酸酯中任意一种或几种组合。
进一步的,一种美白抗初老洁面乳的制备方法,包括以下步骤:
S1、取γ-聚谷氨酸、阿魏酸、沙虫体壁溶出物混合搅拌,获得组分A;
S2、在组分A中加入碧萝芷、活性肽、N-乙酰基-L-鸭皂酸、水杨酰植物鞘胺醇混合搅拌,加入表面活性剂,在-10~-15℃下静置1-3h,得到组分B,备用;
S3、取神经酰胺NP、橄榄苦苷、甘草酸二钾、羧甲基脱乙酰壳多糖混合搅拌得到组分C,备用;
S4、将乳化剂和1,3-丙二醇、印度楝叶提取物、尿囊素混合并加热到74-90℃,均质3-5分钟,得到组分D;
S5、在组分D中加入组分B、组分C和水在7000-10000rpm条件下进行剪切乳化5-8min,得到乳化液,即为美白抗初老洁面乳。
进一步的,所述S1中在避光环境、20-23℃下混合搅拌,搅拌速率为200-400rpm,搅拌时间20-40min。
进一步的,所述S4中均质压力为40-60MPa,温度为30-40℃。
与现有技术相比,本发明的有益效果是:
本发明的洁面乳具有较好的美白效果和抗初老效果,经美白原料、抗氧化原料、具有修复作用的原料和辅料科学配比而成,具有抑制前列腺素及组胺的释放,进而抑制人源表皮黑色素细胞B16的络氨酸酶的活性,抑制黑色素生长,达到美白的效果,且具有较佳的抗氧化活性,高效清除DPPH自由基,使在抑制黑色素的同时,还能降低毛细血管的通透性,抑制血红素,修复屏障,减少皮肤泛红;并且还能通过提高皮肤抗氧化能力减缓皮肤老化的过程,促进皮肤新陈代谢,通过促进皮肤弹性蛋白的表达和细胞的增殖生长改善皮肤初老;另外辅料能够起到保湿补水的作用,
具体实施方式
为了更好理解本发明技术内容,下面提供具体实施例,对本发明做进一步的说明。
本发明实施例所用的实验方法如无特殊说明,均为常规方法。
本发明实施例所用的材料、试剂等,如无特殊说明,均可从商业途径得到。
实施例1
一种美白抗初老洁面乳:包括以下重量份原料:环γ-聚谷氨酸12份、阿魏酸0.3份、沙虫体壁溶出物3份、碧萝芷15份、活性肽2.6份、N-乙酰基-L-鸭皂酸2.5份、水杨酰植物鞘胺醇0.5份、神经酰胺NP5.2份、橄榄苦苷1.9份、甘草酸二钾2.5份、羧甲基脱乙酰壳多糖3.8份、1,3-丙二醇3.8份、印度楝叶提取物1.5份、尿囊素2.6份、表面活性剂3份、乳化剂2份、水25份;
所述活性肽为质量比3.6:1.3:11.5的棕榈酰三肽-5、乙酰基四肽-11、棕榈酰五肽-4;
所述沙虫体壁溶出物是将沙虫放入质量浓度为0.1‰的柠檬酸溶液中浸泡30min,沙虫和柠檬酸溶液的质量体积比g/mL为3:15,80℃下微波加热8min,超声过滤,取液体,在40℃下蒸发浓缩,将浓缩液在-30℃下冷冻干燥,得到,沙虫体壁溶出物。
所述表面活性剂为月桂酸;
所述乳化剂为聚甘油-10二异硬脂酸酯。
实施例2
一种美白抗初老洁面乳:包括以下重量份原料:环γ-聚谷氨酸25份、阿魏酸1.5份、沙虫体壁溶出物5份、碧萝芷50份、活性肽8.9份、N-乙酰基-L-鸭皂酸5.8份、水杨酰植物鞘胺醇1.5份、神经酰胺NP11.9份、橄榄苦苷5.6份、甘草酸二钾5.9份、羧甲基脱乙酰壳多糖5.9份、1,3-丙二醇6.1份、印度楝叶提取物2.8份、尿囊素5.9份、表面活性剂9份、乳化剂6份、水49份;
所述活性肽为质量比8.5:2.8:18.6的棕榈酰三肽-5、乙酰基四肽-11、棕榈酰五肽-4;
所述沙虫体壁溶出物是将沙虫放入质量浓度为0.2‰的柠檬酸溶液中浸泡50min,沙虫和柠檬酸溶液的质量体积比g/mL为8:15,100℃下微波加热15min,超声过滤,取液体,在85℃下蒸发浓缩,将浓缩液在-5℃下冷冻干燥,得到,沙虫体壁溶出物。
所述表面活性剂为棕榈酸;
所述乳化剂为山梨醇聚醚-30四油酸酯。
实施例3
一种美白抗初老洁面乳:包括以下重量份原料:环γ-聚谷氨酸20份、阿魏酸0.9份、沙虫体壁溶出物4份、碧萝芷33份、活性肽6.2份、N-乙酰基-L-鸭皂酸3.7份、水杨酰植物鞘胺醇1.0份、神经酰胺NP8.4份、橄榄苦苷4.1份、甘草酸二钾3.8份、羧甲基脱乙酰壳多糖4.8份、1,3-丙二醇5.2份、印度楝叶提取物2.2份、尿囊素3.1份、表面活性剂7份、乳化剂4份、水37份;
所述活性肽为质量比5.9:2.1:15.6的棕榈酰三肽-5、乙酰基四肽-11、棕榈酰五肽-4;
所述沙虫体壁溶出物是将沙虫放入质量浓度0.‰的柠檬酸溶液中浸泡40min,沙虫和柠檬酸溶液的质量体积比g/mL为5:15,90℃下微波加热11min,超声过滤,取液体,在65℃下蒸发浓缩,将浓缩液在-25℃下冷冻干燥,得到,沙虫体壁溶出物;
所述表面活性剂为肉豆蔻酸;
所述乳化剂为PEG-3二硬脂酸酯;
上述实施例1-3采用以下制备方法:包括以下步骤:
S1、取γ-聚谷氨酸、阿魏酸、沙虫体壁溶出物在避光环境、20-23℃下混合搅拌,搅拌速率为200-400rpm,搅拌时间20-40min,获得组分A;
S2、在组分A中加入碧萝芷、活性肽、N-乙酰基-L-鸭皂酸、水杨酰植物鞘胺醇混合搅拌,加入表面活性剂,在-10~-15℃下静置1-3h,得到组分B,备用;
S3、取神经酰胺NP、橄榄苦苷、甘草酸二钾、羧甲基脱乙酰壳多糖混合搅拌得到组分C,备用;
S4、将乳化剂和1,3-丙二醇、印度楝叶提取物、尿囊素混合并加热到74-90℃,在均质压力为40-60MPa,温度为30-40℃下均质3-5分钟,得到组分D;
S5、在组分D中加入组分B、组分C和水在7000-10000rpm条件下进行剪切乳化5-8min,得到乳化液,即为美白抗初老洁面乳。
实施例4
一种美白抗初老洁面乳:包括以下重量份原料:环γ-聚谷氨酸20份、阿魏酸0.9份、沙虫体壁溶出物4份、碧萝芷33份、活性肽6.2份、N-乙酰基-L-鸭皂酸3.7份、水杨酰植物鞘胺醇1.0份、神经酰胺NP8.4份、橄榄苦苷4.1份、甘草酸二钾3.8份、羧甲基脱乙酰壳多糖4.8份、1,3-丙二醇5.2份、印度楝叶提取物2.2份、尿囊素3.1份、表面活性剂7份、乳化剂4份、水37份;
所述活性肽为质量比5.9:2.1:15.6的棕榈酰三肽-5、乙酰基四肽-11、棕榈酰五肽-4;
所述沙虫体壁溶出物是将沙虫放入质量浓度0.‰的柠檬酸溶液中浸泡40min,沙虫和柠檬酸溶液的质量体积比g/mL为5:15,90℃下微波加热11min,超声过滤,取液体,在65℃下蒸发浓缩,将浓缩液在-25℃下冷冻干燥,得到,沙虫体壁溶出物;
所述表面活性剂为肉豆蔻酸;
所述乳化剂为PEG-3二硬脂酸酯;
上述洁面乳采用以下制备方法:包括以下步骤:
S1、取γ-聚谷氨酸、阿魏酸、沙虫体壁溶出物在避光环境、20℃下混合搅拌,搅拌速率为200rpm,搅拌时间20min,获得组分A;
S2、在组分A中加入碧萝芷、活性肽、N-乙酰基-L-鸭皂酸、水杨酰植物鞘胺醇混合搅拌,加入表面活性剂,在-10℃下静置1h,得到组分B,备用;
S3、取神经酰胺NP、橄榄苦苷、甘草酸二钾、羧甲基脱乙酰壳多糖混合搅拌得到组分C,备用;
S4、将乳化剂和1,3-丙二醇、印度楝叶提取物、尿囊素混合并加热到74℃,在均质压力为40MPa,温度为30℃下均质3分钟,得到组分D;
S5、在组分D中加入组分B、组分C和水在7000rpm条件下进行剪切乳化5min,得到乳化液,即为美白抗初老洁面乳。
实施例5
一种美白抗初老洁面乳:包括以下重量份原料:环γ-聚谷氨酸20份、阿魏酸0.9份、沙虫体壁溶出物4份、碧萝芷33份、活性肽6.2份、N-乙酰基-L-鸭皂酸3.7份、水杨酰植物鞘胺醇1.0份、神经酰胺NP8.4份、橄榄苦苷4.1份、甘草酸二钾3.8份、羧甲基脱乙酰壳多糖4.8份、1,3-丙二醇5.2份、印度楝叶提取物2.2份、尿囊素3.1份、表面活性剂7份、乳化剂4份、水37份;
所述活性肽为质量比5.9:2.1:15.6的棕榈酰三肽-5、乙酰基四肽-11、棕榈酰五肽-4;
所述沙虫体壁溶出物是将沙虫放入质量浓度0.‰的柠檬酸溶液中浸泡40min,沙虫和柠檬酸溶液的质量体积比g/mL为5:15,90℃下微波加热11min,超声过滤,取液体,在65℃下蒸发浓缩,将浓缩液在-25℃下冷冻干燥,得到,沙虫体壁溶出物;
所述表面活性剂为肉豆蔻酸;
所述乳化剂为PEG-3二硬脂酸酯;
上述洁面乳采用以下制备方法:包括以下步骤:
S1、取γ-聚谷氨酸、阿魏酸、沙虫体壁溶出物在避光环境、23℃下混合搅拌,搅拌速率为400rpm,搅拌时间40min,获得组分A;
S2、在组分A中加入碧萝芷、活性肽、N-乙酰基-L-鸭皂酸、水杨酰植物鞘胺醇混合搅拌,加入表面活性剂,在-15℃下静置3h,得到组分B,备用;
S3、取神经酰胺NP、橄榄苦苷、甘草酸二钾、羧甲基脱乙酰壳多糖混合搅拌得到组分C,备用;
S4、将乳化剂和1,3-丙二醇、印度楝叶提取物、尿囊素混合并加热到90℃,在均质压力为60MPa,温度为40℃下均质5分钟,得到组分D;
S5、在组分D中加入组分B、组分C和水在10000rpm条件下进行剪切乳化8min,得到乳化液,即为美白抗初老洁面乳。
对比例1
本对比例与实施例1的区别在于,一种美白抗初老洁面乳,包括以下重量份原料:环γ-聚谷氨酸10份、阿魏酸0.8份、沙虫体壁溶出物9份、碧萝芷10份、活性肽2.1份、N-乙酰基-L-鸭皂酸8.4份、水杨酰植物鞘胺醇2.9份、神经酰胺NP3.1份、橄榄苦苷0.9份、甘草酸二钾7.5份、羧甲基脱乙酰壳多糖2.9份、1,3-丙二醇2.8份、印度楝叶提取物1.0份、尿囊素8.5份、表面活性剂1份、乳化剂9份、水20份。
对比例2
本对比例与实施例3的区别在于,所述美白抗初老洁面乳的原料中不含有沙虫体壁溶出物。
对比例3
本对比例与实施例3的区别在于,所述美白抗初老洁面乳的原料中不含有碧萝芷。
对比例4
本对比例与实施例3的区别在于,所述美白抗初老洁面乳的原料中活性肽为质量比5.9:2.1:15.6的寡肽-1、三肽-1、五肽-1。
一、效果测试:
1、抑制络氨酸酶试验:分别取0.1mL实施例1-5和对比例1-4的洁面乳放置试管中,分别向试管中加入100μL的磷酸盐缓冲溶液,得到混合液,作为实验组,空白组磷酸盐缓冲溶液,备用;选择人源表皮黑色素细胞B16,以1×105密度培养在96孔板中,培养24h后,将试管中混合液分别加样于96孔板中,避光条件下混匀,于35±2℃水浴恒温培养24h,每孔加入含1%TritonX-100的PBS缓冲液100uL,然后加入50uL0.2mg/mL的L-DOPA,37C处理3h后再测定490nm的吸光值。按如下公式计算酶活力:
酪氨酸酶抑制率(%)=[1-(实验组OD值/空白组OD值]×100%。
2、黑色素含量测定:取对数期的人源表皮黑色素细胞B16弃去培养液,用PBS液清洗2次,加入培养液,调节细胞浓度为0.5-1×10个/孔,加入96孔板中,并加入1pM浓度的α-MSH进行黑色素诱导,在37℃下培养24h。细胞贴壁后,弃去原有培养液;实验组为实施例1-5和对比例1-4的洁面乳试管混合液,对照组为α-MSH;空白组为磷酸盐溶液,每个孔的细胞加入100uL含10%二甲基亚砜(DMSO)的Na0H(1mol/L)溶液,于70℃水浴完全溶解黑色素颗粒,检测490nm处吸光度,黑色素含量按照以下计算公式:
黑色素含量减少率(%)=[(实验组OD值-空白组OD值)/(对照组OD值-空白组OD值]×100%;
3、毛细血管通透性能测定:抑制Fltl活性可以降低毛细血管的通透性,取100uLpolyE4Y溶液添加到未经处理的96孔板中在2±1℃下放置12h,添加Fltl酪氨酸激酸(GST-F,100nmol/L)和本发明样品(5g/L)到板上,并且在30±2℃下培养1h。用Tris/NaCl缓冲液清洗板后,室温下用5%BSA封闭30min。用含有0.1%Tween的TrisNaCl缓冲液冲洗孔板,PY20(每个孔100μL,20μg/L)添加到每个板孔中,在室温下培养2h。冲洗该板三次后,添加HRP-IgG(每板孔100μL,40μg/L),然后在室温下培养1h。最后该板用TBST缓冲液冲洗四次。显像缓冲液(100μL,柠檬酸缓冲液0.1mo1/L,pH5.5.H2021.3mmol/L,0-邻苯二胶10mmol/L)添加到每个板孔中。颜色变化后用100uL,lmol/LH2SO4终止反应。在492nm下酶标仪进行检测。
结果如下表:
上述结果可知,本发明的洁面乳有效抑制人源表皮黑色素细胞B16的络氨酸酶的活性,其中沙虫体壁溶出物中的胶原蛋白成分可以通过螯合铜离子来抑制络氨酸酶活性,也可以通过降低细胞内环磷酸腺苷的含量来抑制络氨酸酶的表达,从而抑制黑色素生长,具有较佳的抗氧化活性,酪氨酸酶抑制率90.1-93.8%,黑色素含量减少率95.1-98.4%,Fltl抑制率84.2-89.7%,则可说明有效降低毛细血管的通透性,在抑制黑色素的同时,
二、抗初老效果测试
1、清除DPPH自由基活性测定:分别取本发明洁面乳实施例1-5和对比例1-4的样品各1.0g,加入1.52×10-4mmol/L的DPPH无水乙醇溶液2mL充分混匀,室温避光静置30min后,以溶剂为空白对照,517nm处测吸光度A1;以同体积溶剂代替样品溶液做阴性对照,测定吸光度A2;以同体积无水乙醇代替DPPH溶液做空白组,测定吸光度A3,以VC为对照,每组做3个重复,求其平均值,按下式计算清除率:
DPPH的清除率(%)=[1-(A1-A3)/A2]×100%
2、基质金属蛋白酶表达抑制率:将成纤维细胞接种到24孔细胞培养板每个孔含有0.5×105个细胞,饥饿培养24h。用PBS冲洗并且用蓝光照射处理。然后,在48h内,向细胞中加入本发明洁面乳样品1-2次。测量培养基中分离的MMP-1。通过计算MMP-12的表达抑制率;抑制率公式如下:
抑制率%=(A0-A1)/A0×100%;
A0为经蓝光照射后,但未添加样品的MMP-1的表达量,A1为经蓝光照射后,且添加本实施例中样品的MMP-1的表达量。
3、弹性蛋白酶活性抑制率:在96孔板调制成10mg/L三羟甲基氨基甲烷盐酸盐缓冲液混合200uI的各测试样品及50uL的20ug/mL弹性蛋白酶-III型溶液。将250uM的EGCG作为阳性对照组来使用,并且作为阴性对照组的非处理组使用了蒸馏水,并且在25℃下反应50min。测定415nm波长下的吸光度;抑制率计算公式如下:
弹性蛋白酶活性抑制率(%)=[1-(样品添加试剂吸光度-样品添加试剂对照吸光度)/(样品未添加试剂吸光度-样品未添加试剂对照吸光度)]×100%
结果如下表:
由上述结果可知,本发明的洁面乳具有一定的抗氧化效果,抑制MMP-12金属蛋白酶的表达,有效抑制弹性蛋白酶,其中DPPH清除率为64.2-69.4%,MMP-12金属蛋白酶抑制率为60.4-68.8%,弹性蛋白酶抑制率为90.1-92.3%。
实施例组与对比例1比较,说明各原料按特定的比例混合,能达到较好的抗氧化、弹性蛋白酶抑制、抗老化等作用效果;
实施例组与对比例3、4比较,碧萝芷具有较佳的抗氧化性能,通过提高皮肤抗氧化能力减缓皮肤老化的过程,通过促进皮肤弹性蛋白的表达和细胞的增殖生长改善皮肤初老。活性肽经棕榈酰三肽-5、乙酰基四肽-11、棕榈酰五肽-4的复配,具有清除细胞外基质降解的作用,同时能够刺激细胞基质中胶原蛋白和弹性蛋白生成,从而达到抗光老化的作用,而且三螺旋结构能强劲锁住水分,让皮肤时刻保持湿润、水嫩,在蓝光处理下有效减少活性氧产生,减少外界环境导致的皮肤老化现象。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (5)
1.一种美白抗初老洁面乳,其特征在于:包括以下重量份原料:环γ-聚谷氨酸12-25份、阿魏酸0.3-1.5份、沙虫体壁溶出物3-5份、碧萝芷15-50份、活性肽2.6-8.9份、N-乙酰基-L-鸭皂酸2.5-5.8份、水杨酰植物鞘胺醇0.5-1.5份、神经酰胺NP5.2-11.9份、橄榄苦苷1.9-5.6份、甘草酸二钾2.5-5.9份、羧甲基脱乙酰壳多糖3.8-5.9份、1,3-丙二醇3.8-6.1份、印度楝叶提取物1.5-2.8份、尿囊素2.6-5.9份、表面活性剂3-9份、乳化剂2-6份、水25-49份;所述活性肽为质量比(3.6-8.5):(1.3-2.8):(11.5-18.6)的棕榈酰三肽-5、乙酰基四肽-11、棕榈酰五肽-4;所述沙虫体壁溶出物是将沙虫放入质量浓度为0.1-0.2‰的柠檬酸溶液中浸泡30-50min,沙虫和柠檬酸溶液的质量体积比g/mL为3-8:15,80-100℃下微波加热8-15min,超声过滤,取液体,在40-85℃下蒸发浓缩,将浓缩液在-30~-5℃下冷冻干燥,得到,沙虫体壁溶出物;所述表面活性剂为肉豆蔻酸、月桂酸、棕榈酸、甲基椰油酰基牛磺酸钠、月桂基葡糖苷中任意一种或几种组合;所述乳化剂为PEG-3二硬脂酸酯、山梨醇聚醚-30四油酸酯、聚甘油-10二异硬脂酸酯中任意一种或几种组合。
2.如权利要求1所述的一种美白抗初老洁面乳,其特征在于:包括以下重量份原料:环γ-聚谷氨酸20份、阿魏酸0.9份、沙虫体壁溶出物4份、碧萝芷33份、活性肽6.2份、N-乙酰基-L-鸭皂酸3.7份、水杨酰植物鞘胺醇1.0份、神经酰胺NP8.4份、橄榄苦苷4.1份、甘草酸二钾3.8份、羧甲基脱乙酰壳多糖4.8份、1,3-丙二醇5.2份、印度楝叶提取物2.2份、尿囊素3.1份。
3.如权利要求1所述的一种美白抗初老洁面乳的制备方法,其特征在于:包括以下步骤:
S1、取γ-聚谷氨酸、阿魏酸、沙虫体壁溶出物混合搅拌,获得组分A;
S2、在组分A中加入碧萝芷、活性肽、N-乙酰基-L-鸭皂酸、水杨酰植物鞘胺醇混合搅拌,加入表面活性剂,在-10~-15℃下静置1-3h,得到组分B,备用;
S3、取神经酰胺NP、橄榄苦苷、甘草酸二钾、羧甲基脱乙酰壳多糖混合搅拌得到组分C,备用;
S4、将乳化剂和1,3-丙二醇、印度楝叶提取物、尿囊素混合并加热到74-90℃,均质3-5分钟,得到组分D;
S5、在组分D中加入组分B、组分C和水在7000-10000rpm条件下进行剪切乳化5-8min,得到乳化液,即为美白抗初老洁面乳。
4.如权利要求3所述的一种美白抗初老洁面乳的制备方法,其特征在于:所述S1中在避光环境、20-23℃下混合搅拌,搅拌速率为200-400rpm,搅拌时间20-40min。
5.如权利要求3所述的一种美白抗初老洁面乳的制备方法,其特征在于:所述S4中均质压力为40-60MPa,温度为30-40℃。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202311158058.4A CN117017831B (zh) | 2023-09-08 | 2023-09-08 | 一种美白抗初老洁面乳及其制备工艺 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202311158058.4A CN117017831B (zh) | 2023-09-08 | 2023-09-08 | 一种美白抗初老洁面乳及其制备工艺 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN117017831A CN117017831A (zh) | 2023-11-10 |
CN117017831B true CN117017831B (zh) | 2024-03-19 |
Family
ID=88643244
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202311158058.4A Active CN117017831B (zh) | 2023-09-08 | 2023-09-08 | 一种美白抗初老洁面乳及其制备工艺 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN117017831B (zh) |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102784084A (zh) * | 2012-08-22 | 2012-11-21 | 珀莱雅(湖州)化妆品有限公司 | 皮肤抗老化脂质纳米粒乳液及其制备方法 |
CN106474041A (zh) * | 2016-12-11 | 2017-03-08 | 钦州学院 | 一种用沙虫粉制成的面膜霜 |
KR20220118660A (ko) * | 2021-02-19 | 2022-08-26 | 나인바이오팜 주식회사 | 천연 추출물을 포함하는 미백 화장료 조성물 |
CN115381727A (zh) * | 2022-09-27 | 2022-11-25 | 广州森野生物医药科技有限公司 | 一种美白祛斑组合物及其制备方法 |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20040166069A1 (en) * | 2003-02-21 | 2004-08-26 | Gupta Shyam K. | Boosting Tyrosinase Inhibiting Activity of Skin Whitening and Sunscreen Compositions |
US20080254130A1 (en) * | 2003-08-29 | 2008-10-16 | Bioderm Research | Skin Antiaging & Brightening via Multi-function Treatment of Enzyme Dysfunction |
-
2023
- 2023-09-08 CN CN202311158058.4A patent/CN117017831B/zh active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102784084A (zh) * | 2012-08-22 | 2012-11-21 | 珀莱雅(湖州)化妆品有限公司 | 皮肤抗老化脂质纳米粒乳液及其制备方法 |
CN106474041A (zh) * | 2016-12-11 | 2017-03-08 | 钦州学院 | 一种用沙虫粉制成的面膜霜 |
KR20220118660A (ko) * | 2021-02-19 | 2022-08-26 | 나인바이오팜 주식회사 | 천연 추출물을 포함하는 미백 화장료 조성물 |
CN115381727A (zh) * | 2022-09-27 | 2022-11-25 | 广州森野生物医药科技有限公司 | 一种美白祛斑组合物及其制备方法 |
Also Published As
Publication number | Publication date |
---|---|
CN117017831A (zh) | 2023-11-10 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US10117821B2 (en) | Topical lightening composition and methods of use thereof | |
KR101578342B1 (ko) | 주름을 방지 또는 개선하기 위한 경구, 주사, 피부 외용제 및 미용 방법 | |
US6723688B1 (en) | Cleanser that is gentle to human skin | |
CN112494406A (zh) | 一种美白祛斑化妆品及其制备方法 | |
CN111281840B (zh) | 一种亮颜美肤霜及其制备方法 | |
CN109464295A (zh) | 一种含低分子量岩藻寡糖的皮肤护理组合物 | |
CN105411951A (zh) | 黑柄炭角菌提取物在美白保湿化妆品中的应用 | |
CN102274141A (zh) | 复活草水活保湿霜及其制备方法 | |
JP2001163754A (ja) | 老化防止剤及びこれを配合した化粧料 | |
KR102373899B1 (ko) | 피부의 주름 개선, 미백, 세포 재생, 상처 치유에 유효한 복합 천연물 추출물을 활성성분으로 함유하는 다 기능성 화장품 조성물 | |
CN108852969B (zh) | 一种抗皱抗衰老美白面膜及其制备方法 | |
CN117017831B (zh) | 一种美白抗初老洁面乳及其制备工艺 | |
CN111110581B (zh) | 具有提高美白功能的新琼寡糖组合物及其应用 | |
KR100834891B1 (ko) | 두족류의 먹물추출물을 포함하는 모발 처리제 조성물. | |
CN111012713B (zh) | 美白组合物及其制备方法和用途 | |
CN101357114A (zh) | 美白抗氧化化妆组合物 | |
JP2004231558A (ja) | 美白用皮膚外用剤 | |
JPH10287528A (ja) | 化粧料組成物 | |
KR102291780B1 (ko) | 천연 유래 물질을 포함하는 피부 노화 예방 및 상처 치유용 기능성 화장료 조성물 및 이의 제조방법 | |
CN109528541A (zh) | 一种含五矿多元酵母络合多肽的洗涤组合物 | |
CN115414293A (zh) | 一种抗衰老组合物及其应用 | |
CN114681358A (zh) | 一种酪氨酸酶活性抑制剂及具有增效美白作用的护肤品 | |
CN114469808A (zh) | 一种含酵母肽的抗氧化纳米乳制备方法及在化妆品中的应用 | |
CN108703926A (zh) | 美白保湿紧致抗皱面霜及其制备方法 | |
CN110354053A (zh) | 一种婴儿椰子油洗发沐浴露及其制备方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |