CN117695168B - Composition with anti-aging repairing effect, freeze-dried powder and preparation method and application thereof - Google Patents
Composition with anti-aging repairing effect, freeze-dried powder and preparation method and application thereof Download PDFInfo
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- CN117695168B CN117695168B CN202410158300.6A CN202410158300A CN117695168B CN 117695168 B CN117695168 B CN 117695168B CN 202410158300 A CN202410158300 A CN 202410158300A CN 117695168 B CN117695168 B CN 117695168B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000000203 mixture Substances 0.000 title claims abstract description 30
- 230000003712 anti-aging effect Effects 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 title claims abstract description 21
- 230000000694 effects Effects 0.000 title claims abstract description 20
- 239000000284 extract Substances 0.000 claims abstract description 29
- IHRKJQSLKLYWBQ-QKDODKLFSA-N (2s)-2-[[(2s)-1-[(2s)-5-amino-2-[[2-(hexadecanoylamino)acetyl]amino]-5-oxopentanoyl]pyrrolidine-2-carbonyl]amino]-5-(diaminomethylideneamino)pentanoic acid Chemical compound CCCCCCCCCCCCCCCC(=O)NCC(=O)N[C@@H](CCC(N)=O)C(=O)N1CCC[C@H]1C(=O)N[C@@H](CCCN=C(N)N)C(O)=O IHRKJQSLKLYWBQ-QKDODKLFSA-N 0.000 claims abstract description 14
- SSISHJJTAXXQAX-ZETCQYMHSA-N L-ergothioneine Chemical compound C[N+](C)(C)[C@H](C([O-])=O)CC1=CNC(=S)N1 SSISHJJTAXXQAX-ZETCQYMHSA-N 0.000 claims abstract description 14
- 229940093497 ergothioneine Drugs 0.000 claims abstract description 14
- 229940094946 palmitoyl tetrapeptide-7 Drugs 0.000 claims abstract description 14
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims abstract description 13
- 229930195725 Mannitol Natural products 0.000 claims abstract description 13
- 235000010355 mannitol Nutrition 0.000 claims abstract description 13
- 239000000594 mannitol Substances 0.000 claims abstract description 13
- LHGVFZTZFXWLCP-UHFFFAOYSA-N guaiacol Chemical compound COC1=CC=CC=C1O LHGVFZTZFXWLCP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229960001855 mannitol Drugs 0.000 claims abstract description 8
- 239000002537 cosmetic Substances 0.000 claims abstract description 7
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims abstract description 7
- UBFRDALTOGELDQ-UHFFFAOYSA-L manganese(2+) 2-methoxyphenol dichloride Chemical compound [Cl-].[Mn+2].C=1(C(O)=CC=CC1)OC.[Cl-] UBFRDALTOGELDQ-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims abstract description 5
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229940099607 manganese chloride Drugs 0.000 claims abstract description 5
- 235000002867 manganese chloride Nutrition 0.000 claims abstract description 5
- 239000011565 manganese chloride Substances 0.000 claims abstract description 5
- 229960001867 guaiacol Drugs 0.000 claims abstract description 4
- 239000008176 lyophilized powder Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 229940091557 ethylbisiminomethylguaiacol manganese chloride Drugs 0.000 claims description 16
- YUZJJFWCXJDFOQ-UHFFFAOYSA-K manganese(3+);2-methoxy-6-[2-[(3-methoxy-2-oxidophenyl)methylideneamino]ethyliminomethyl]phenolate;chloride Chemical compound [Cl-].[Mn+3].COC1=CC=CC(C=NCCN=CC=2C(=C(OC)C=CC=2)[O-])=C1[O-] YUZJJFWCXJDFOQ-UHFFFAOYSA-K 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 13
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical class O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 241001186295 Lespedeza capitata Species 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 10
- 235000014037 Castanea sativa Nutrition 0.000 claims description 9
- 240000007857 Castanea sativa Species 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001694 spray drying Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 6
- 238000000638 solvent extraction Methods 0.000 claims description 6
- KQXNSIFXSLHNSG-UHFFFAOYSA-L [Cl-].C(C)C1=C(C(=C(C(=C1)OC)O)C=N)C=N.[Mn+2].[Cl-] Chemical compound [Cl-].C(C)C1=C(C(=C(C(=C1)OC)O)C=N)C=N.[Mn+2].[Cl-] KQXNSIFXSLHNSG-UHFFFAOYSA-L 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- PCWPQSDFNIFUPO-VDQKLNDWSA-N (1S,3R,5R,6S,8R,10R,11S,13R,15R,16S,18R,20R,21S,23R,25R,26S,28R,30R,31S,33R,35R,36R,37S,38R,39S,40R,41S,42R,43S,44R,45S,46R,47S,48R,49S)-37,39,41,43,45,47,49-heptakis(2-hydroxyethoxy)-5,10,15,20,25,30,35-heptakis(hydroxymethyl)-2,4,7,9,12,14,17,19,22,24,27,29,32,34-tetradecaoxaoctacyclo[31.2.2.23,6.28,11.213,16.218,21.223,26.228,31]nonatetracontane-36,38,40,42,44,46,48-heptol Chemical compound OCCO[C@H]1[C@H](O)[C@@H]2O[C@H]3O[C@H](CO)[C@@H](O[C@H]4O[C@H](CO)[C@@H](O[C@H]5O[C@H](CO)[C@@H](O[C@H]6O[C@H](CO)[C@@H](O[C@H]7O[C@H](CO)[C@@H](O[C@H]8O[C@H](CO)[C@@H](O[C@H]1O[C@@H]2CO)[C@@H](O)[C@@H]8OCCO)[C@@H](O)[C@@H]7OCCO)[C@@H](O)[C@@H]6OCCO)[C@@H](O)[C@@H]5OCCO)[C@@H](O)[C@@H]4OCCO)[C@@H](O)[C@@H]3OCCO PCWPQSDFNIFUPO-VDQKLNDWSA-N 0.000 claims description 2
- ODLHGICHYURWBS-LKONHMLTSA-N trappsol cyclo Chemical compound CC(O)COC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)COCC(O)C)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1COCC(C)O ODLHGICHYURWBS-LKONHMLTSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 230000000052 comparative effect Effects 0.000 description 10
- 239000002994 raw material Substances 0.000 description 5
- 229940083957 1,2-butanediol Drugs 0.000 description 4
- BMRWNKZVCUKKSR-UHFFFAOYSA-N butane-1,2-diol Chemical compound CCC(O)CO BMRWNKZVCUKKSR-UHFFFAOYSA-N 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 229920000858 Cyclodextrin Polymers 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 241000522169 Lespedeza Species 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 102000016387 Pancreatic elastase Human genes 0.000 description 3
- 108010067372 Pancreatic elastase Proteins 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- -1 hydroxy cyclodextrin Chemical compound 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000003796 beauty Effects 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 230000009759 skin aging Effects 0.000 description 2
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 1
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 1
- 229940035437 1,3-propanediol Drugs 0.000 description 1
- IUVCFHHAEHNCFT-INIZCTEOSA-N 2-[(1s)-1-[4-amino-3-(3-fluoro-4-propan-2-yloxyphenyl)pyrazolo[3,4-d]pyrimidin-1-yl]ethyl]-6-fluoro-3-(3-fluorophenyl)chromen-4-one Chemical compound C1=C(F)C(OC(C)C)=CC=C1C(C1=C(N)N=CN=C11)=NN1[C@@H](C)C1=C(C=2C=C(F)C=CC=2)C(=O)C2=CC(F)=CC=C2O1 IUVCFHHAEHNCFT-INIZCTEOSA-N 0.000 description 1
- KVKVGRLZWBISKU-UHFFFAOYSA-N C(C)C1=C(C(=C(C(=C1)OC)O)C=N)C=N Chemical compound C(C)C1=C(C(=C(C(=C1)OC)O)C=N)C=N KVKVGRLZWBISKU-UHFFFAOYSA-N 0.000 description 1
- 102000016942 Elastin Human genes 0.000 description 1
- 108010014258 Elastin Proteins 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000001153 anti-wrinkle effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 229940059958 centella asiatica extract Drugs 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 229920002549 elastin Polymers 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 229940093476 ethylene glycol Drugs 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 210000002950 fibroblast Anatomy 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 238000011005 laboratory method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—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
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0216—Solid or semisolid forms
- A61K8/022—Powders; Compacted Powders
-
- 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
- A61K8/49—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
- A61K8/58—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing atoms other than carbon, hydrogen, halogen, oxygen, nitrogen, sulfur or phosphorus
-
- 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
- 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
-
- 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
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/84—Products or compounds obtained by lyophilisation, freeze-drying
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Dermatology (AREA)
- Emergency Medicine (AREA)
- Cosmetics (AREA)
Abstract
The invention relates to the technical field of cosmetics, in particular to a composition with an anti-aging repairing effect, freeze-dried powder and a preparation method and application thereof, wherein the composition contains ethyl diiminomethyl guaiacol manganese chloride supermolecule, ergothioneine, palmitoyl tetrapeptide-7, mannitol and an extract composition; the content of the manganese chloride supermolecule of the ethyldiiminomethyl guaiacol is 0.1 to 1 part by weight, the content of the ergothioneine is 0.1 to 1 part by weight, the content of the palmitoyl tetrapeptide-7 is 0.1 to 1 part by weight, and the content of the extract combination is 1 to 10 parts by weight, relative to 100 parts by weight of the mannitol. The freeze-dried powder prepared by the invention has excellent anti-aging performance.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to a composition with an anti-aging repairing effect, freeze-dried powder and a preparation method and application thereof.
Background
The skin is positioned on the outermost layer of the body and is directly contacted with the external environment, so that the external stimulus such as microbial invasion, chemical component harm, ultraviolet injury and the like can be prevented, and the skin is a first defense line of the body. Due to natural age, insufficient daily care, improper or excessive use of cosmetics, transitional fatigue, various accidents and other factors, many people have the phenomenon of premature skin aging.
Various means have been employed to mask and treat this aging. Most of the products on the market at present are traditional cosmetic formulations, such as water cream, and the products of the formulations often cannot protect the activity of functional raw materials in the formula, so that the efficacy of the products is greatly reduced.
The freeze-dried powder is a formulation product newly added in the beauty industry in recent years, and is the development and application of biological freeze-drying technology in the beauty industry.
CN112773726a discloses an ethyl bis iminomethyl guaiacol manganese chloride freeze-dried powder, which comprises the following raw materials in percentage by weight: 5-8 parts of excipient; 0.05-0.6 of protective agent; 0.05-0.2 of ethyl bis iminomethyl guaiacol manganese chloride; 0.2 to 0.8 percent of solubilizer; 0.06-0.15 parts of buffer; centella asiatica extract 0.3 and the balance deionized water. The pH range of the freeze-dried powder obtained by the technical scheme is 6.0-8.0 after rehydration and dissolution, the freeze-dried powder is convenient to use, has good skin feel, protects the activity of the ethyl bis iminomethyl guaiacol manganese chloride, and can be stored for a long time. However, the active ingredients of the scheme are relatively single, and other active matters are required to be compounded in actual use to achieve better anti-aging effect.
Therefore, the development of the freeze-dried powder type with remarkable anti-aging effect and capability of protecting the activity of the functional raw materials of the product for a long time has important practical significance.
Disclosure of Invention
The invention aims to overcome the defect of poor anti-aging performance of the existing anti-aging products in the forms of water cream and the like.
In order to achieve the above object, a first aspect of the present invention provides a lyophilized powder composition having an anti-aging and repairing effect, wherein the composition comprises an ethyl bis iminomethyl guaiacol manganese chloride supermolecule, ergothioneine, palmitoyl tetrapeptide-7, mannitol, and an extract combination;
The composition of the extracts comprises the following components in percentage by weight: 0.5-1 of a product obtained by extracting lespedeza capitata and Castanea sativa leaves with a solvent;
the content of the manganese chloride supermolecule of the ethyldiiminomethyl guaiacol is 0.1 to 1 part by weight, the content of the ergothioneine is 0.1 to 1 part by weight, the content of the palmitoyl tetrapeptide-7 is 0.1 to 1 part by weight, and the content of the extract combination is 1 to 10 parts by weight, relative to 100 parts by weight of the mannitol.
The second aspect of the present invention provides a method for preparing lyophilized powder with anti-aging and repairing effects, which is performed by using the components in the lyophilized powder composition described in the first aspect, and comprises the following steps:
(1) Preparation of extract combinations: the weight ratio of the dosage is 1: extracting Lespedeza capitata of 0.5-1 with solvent to obtain the extract combination;
(2) Mixing ethyl diiminomethyl guaiacol manganese chloride supermolecule, ergothioneine, palmitoyl tetrapeptide-7, mannitol and the extract combination in the presence of water to obtain a material I;
(3) And freeze-drying the material I to obtain the freeze-dried powder.
In a third aspect, the present invention provides lyophilized powder with anti-aging and repairing effects prepared by the method described in the second aspect.
A fourth aspect of the present invention provides the use of the lyophilized powder of the third aspect in a skin cosmetic.
Through the technical scheme, the scheme provided by the invention has at least the following advantages:
(1) The freeze-dried powder in the scheme can better preserve and slowly release the activity of the freeze-dried powder, and the application efficiency is greatly improved.
(2) The freeze-dried powder has better anti-aging effect and better wrinkle-removing effect through the compound use of the components.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In the present invention, room temperature represents 25.+ -. 2 ℃ unless otherwise stated.
As described above, the first aspect of the present invention provides a lyophilized powder composition having an anti-aging effect, which comprises an ethyl bis iminomethyl guaiacol manganese chloride supermolecule, ergothioneine, palmitoyl tetrapeptide-7, mannitol, and an extract combination;
The composition of the extracts comprises the following components in percentage by weight: 0.5-1 of a product obtained by extracting lespedeza capitata and Castanea sativa leaves with a solvent;
the content of the manganese chloride supermolecule of the ethyldiiminomethyl guaiacol is 0.1 to 1 part by weight, the content of the ergothioneine is 0.1 to 1 part by weight, the content of the palmitoyl tetrapeptide-7 is 0.1 to 1 part by weight, and the content of the extract combination is 1 to 10 parts by weight, relative to 100 parts by weight of the mannitol.
Preferably, the solvent in the solvent extraction is selected from at least one of water, methanol, ethanol, ethylene glycol, 1, 3-propanediol, and 1, 2-butanediol.
Preferably, the solvent in the solvent extraction is a solvent with a volume ratio of 10:1-4, and ethanol, the inventors of the present invention found that, in this preferred case, the solution of the present invention is capable of improving the anti-aging repair effect and wrinkle-removing effect of the lyophilized powder.
As described above, the second aspect of the present invention provides a method for preparing a lyophilized powder having an anti-aging effect, which is performed by using the components of the lyophilized powder composition described in the first aspect, and comprises:
(1) Preparation of extract combinations: the weight ratio of the dosage is 1: extracting Lespedeza capitata of 0.5-1 with solvent to obtain the extract combination;
(2) Mixing ethyl diiminomethyl guaiacol manganese chloride supermolecule, ergothioneine, palmitoyl tetrapeptide-7, mannitol and the extract combination in the presence of water to obtain a material I;
(3) And freeze-drying the material I to obtain the freeze-dried powder.
Preferably, in step (1), the solvent is used in an amount of 100-200mL relative to 1g of the total amount of the lespedeza capitata and the castanea sativa leaves.
Preferably, the purity of the Castanea sativa leaf is 70-80wt% and the water content is 15-25wt%.
Preferably, the purity of the lespedeza is 75-85wt% and the water content is 10-20wt%.
Preferably, in step (1), the extraction site of the lespedeza is selected from the leaves and/or stems of the lespedeza.
Preferably, in step (1), the conditions of the solvent extraction include: the temperature is 50-80deg.C, and the time is 20-40min.
According to a preferred embodiment, in step (1), the method further comprises grinding the lespedeza capitata and the castanea sativa leaves, sieving with a 100-200 mesh chinese standard sieve, taking off the sieved material, and then carrying out the solvent extraction.
Preferably, in step (1), the method further comprises, after the solvent extraction, sequentially centrifuging and filtering to obtain a centrifugate, and mixing the centrifugate with 1, 2-butanediol to obtain the extract combination.
Preferably, the ratio of the centrifugal liquid to the 1, 2-butanediol is 1:0.1-0.4. The inventor of the present invention found that in this preferred case, the solution of the present invention can improve the anti-aging and repairing effects and the wrinkle-removing effects of the lyophilized powder.
Preferably, the centrifugation is ultrasonic centrifugation.
Preferably, the conditions of the ultrasonic centrifugation include: the frequency is 20-30KHz, the rotating speed is 12000-15000rpm, and the time is 30-45min.
Preferably, in the step (2), the amount of the ethyldiiminomethyl guaiacol manganese chloride supermolecule is 0.1 to 1 part by weight, the amount of the ergothioneine is 0.1 to 1 part by weight, the amount of the palmitoyl tetrapeptide-7 is 0.1 to 1 part by weight, and the amount of the extract combination is 1 to 10 parts by weight, relative to 100 parts by weight of the mannitol.
Preferably, in step (2), the water is used in an amount such that the components of the lyophilized powder composition are completely dissolved.
In step (2) of the present invention, the mixing may be performed by a procedure known in the art, and the present invention is not particularly limited thereto, and for example, may be performed by stirring at room temperature until all the components in the composition are dissolved in the water. And will not be described in detail herein, those skilled in the art should not be construed as limiting the invention.
It should be noted that the post-treatment step in step (2) of the present invention may be performed by using operations known in the art, and the present invention is not particularly limited thereto, for example, may be performed by using a filter sterilization method, which is not described herein, and those skilled in the art should not understand that the present invention is limited thereto.
Preferably, in step (3), the lyophilization conditions include: the temperature is between-50 ℃ and-30 ℃ and the time is between 2 and 5 hours.
Preferably, in step (3), the lyophilization conditions further comprise: the vacuum degree is less than-0.06 MPa.
Preferably, in step (3), the method further comprises, prior to said lyophilization, filling said material I and then performing said lyophilization.
According to a preferred embodiment, a method for preparing a lyophilized powder having an anti-aging and repairing effect, the method further comprises preparing the manganese chloride supermolecule of ethylbis iminomethyl guaiacol by an operation comprising the steps of:
And (3) carrying out first stirring on the cyclodextrin derivative and the ethyl bis (iminomethyl) guaiacol manganese chloride, and then carrying out first spray drying to obtain the ethyl bis (iminomethyl) guaiacol manganese chloride supermolecule.
Preferably, the cyclodextrin derivative is at least one selected from the group consisting of hydroxy cyclodextrin and methyl cyclodextrin.
More preferably, the hydroxy cyclodextrin is at least one selected from hydroxypropyl beta cyclodextrin and hydroxyethyl beta cyclodextrin.
Preferably, the first stirring conditions include: the time is 1-3h, and the temperature is 70-90 ℃.
Preferably, the conditions of the first spray drying include: the temperature is 110-130 ℃, and the sample injection speed is 10-20mL/min.
Preferably, the first spray drying is performed under a protective atmosphere selected from at least one of nitrogen, argon, and helium.
Preferably, the weight ratio of the cyclodextrin derivative to the ethyl bis iminomethyl guaiacol manganese chloride is 1:0.1-0.5.
According to a preferred embodiment, the method further comprises first dissolving the cyclodextrin derivative in water before the first stirring is performed, and then performing the first stirring.
Preferably, the first dissolution conditions include: the time is 0.5-1h, and the temperature is 20-50 ℃.
Preferably, the water is used in an amount of 20-30mL relative to 0.1g of the cyclodextrin derivative.
As described above, the third aspect of the present invention provides a lyophilized powder having an anti-aging and repairing effect prepared by the method of the second aspect.
As described above, a fourth aspect of the present invention provides the use of the lyophilized powder described in the third aspect in a skin cosmetic.
The invention will be described in detail below by way of examples. In the following examples, unless otherwise specified, various materials and instruments were used as commercial products, and specific sources of the materials are shown in Table 1.
TABLE 1
Preparation A was used to prepare manganese chloride ethyl bis iminomethyl guaiacol supermolecule.
Preparation example A1
After 0.5g of cyclodextrin derivative I was first dissolved in 100mL of water (time: 1h, temperature: 25 ℃ C.), 0.2g of ethyl bis iminomethyl guaiacol manganese chloride was added thereto, followed by first stirring and first spray drying in this order, to prepare ethyl bis iminomethyl guaiacol manganese chloride supermolecule F1.
Conditions of the first stirring: the time was 2h and the temperature was 80 ℃.
Conditions of the first spray drying: the temperature is 120 ℃, the sample injection speed is 12mL/min, and the nitrogen atmosphere is adopted.
Preparation example A2
After 0.5g of cyclodextrin derivative I was first dissolved in 135mL of water (time: 0.75h, temperature: 40 ℃ C.), 0.1g of ethyl bis iminomethyl guaiacol manganese chloride was added thereto, followed by first stirring and first spray drying, to prepare ethyl bis iminomethyl guaiacol manganese chloride supermolecule F2.
Conditions of the first stirring: the time was 1.2h and the temperature was 90 ℃.
Conditions of the first spray drying: the temperature is 130 ℃, the sample injection speed is 20mL/min, and the nitrogen atmosphere is adopted.
Preparation example A3
This preparation was conducted in a similar manner to preparation A1 except that in this comparative preparation, an equal mass of cyclodextrin derivative II was used in place of cyclodextrin derivative I in preparation A1 to prepare an ethylbis-iminomethyl guaiacol manganese chloride supermolecule F3.
Preparation example A4
This preparation was conducted in a similar manner to preparation A1 except that 0.3g of ethyl bis iminomethyl guaiacol manganese chloride used in the preparation of this comparative example was used to prepare ethyl bis iminomethyl guaiacol manganese chloride supermolecule F4.
Preparation B was used to prepare the extract combination.
Preparation example B1
Extracting caulis Seu folium Lespedezae Bicoloris and Castanea sativa (both are undersize materials which have passed through 100 mesh Chinese standard sieve), centrifuging with ultrasonic wave, filtering to obtain centrifugate, and adding 1, 2-butanediol to obtain extract composition Z1;
unless otherwise specified, the remaining preparation examples were carried out with reference to the process of preparation example B1, except that the raw materials and process parameters used in each preparation example were not identical, specifically with reference to the cases listed in table 2.
TABLE 2
Preparation example B3
This preparation was conducted in a similar manner to preparation B1, except that in this preparation, the amount of water was adjusted to 100mL and the amount of ethanol was adjusted to 50mL, while keeping the total amount of the solvent unchanged, to prepare an extract composition Z3.
Comparative preparation example DB-1
This comparative preparation was conducted in a similar manner to preparation 1 except that the extract composition D-Z1 was prepared by adjusting the amount of Lespedeza capitata to 0.7g and the amount of Castanea sativa to 0.3g, while keeping the total amount of Lespedeza capitata and Castanea sativa unchanged.
The amounts of the components in the examples below were 1g per part by weight or per part unless otherwise specified.
Example 1
(1) In the presence of water, combining ethyl diiminomethyl guaiacol manganese chloride supermolecule, ergothioneine, palmitoyl tetrapeptide-7, mannitol and extract, stirring and mixing at room temperature until all components in the composition are dissolved in water to obtain a material I;
(2) And (3) filling the material I, and freeze-drying to obtain freeze-dried powder.
The remaining examples were carried out with reference to the process of example 1, without any particular explanation, except that the raw material formulation, amounts and process parameters used in each example were varied, see in particular the cases listed in table 3.
TABLE 3 Table 3
Example 4
This example was conducted in a similar manner to example 1 except that in this example, an equal weight part of ethyl bis iminomethyl guaiacol manganese chloride supermolecule F3 was used in place of F1 in example 1 to prepare a lyophilized powder M4.
Example 5
This example was conducted in a similar manner to example 1 except that in this example, an equal weight part of ethyl bis iminomethyl guaiacol manganese chloride supermolecule F4 was used in place of F1 in example 1 to prepare a lyophilized powder M5.
Example 6
This example was conducted in a similar manner to example 1 except that the same parts by weight of the extract combination Z3 was used in place of Z1 in example 1 in this example to prepare a lyophilized powder M6.
Comparative example 1
This comparative example was conducted in a similar manner to example 1 except that the same weight part of the extract combination D-Z1 was used in place of Z1 in example 1 to prepare lyophilized powder D-M1.
Comparative example 2
This comparative example was conducted in a similar manner to example 1 except that ergothioneine was added in an amount of 1.2 parts by weight to prepare lyophilized powder D-M2.
Comparative example 3
This comparative example was conducted in a similar manner to example 1 except that palmitoyl tetrapeptide-7 was not added thereto to obtain lyophilized powder D-M3.
Test case
The anti-aging efficacy is characterized by evaluating the inhibition rate of elastase by the test sample. Elastase is secreted by fibroblasts and is capable of degrading elastin in the skin leading to skin aging.
Test methods reference laboratory methods (HMC-WI-028 elastase inhibition), and specific results are shown in Table 4.
TABLE 4 Table 4
As can be seen from the results in Table 4, the freeze-dried powder provided by the invention has better anti-aging performance and anti-wrinkle effect.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (8)
1. A freeze-dried powder composition with an anti-aging and repairing effect is characterized in that the composition contains ethyl diiminomethyl guaiacol manganese chloride supermolecule, ergothioneine, palmitoyl tetrapeptide-7, mannitol and an extract composition;
The extract composition comprises the following components in percentage by weight: 0.5-1 of a product obtained by extracting lespedeza capitata and Castanea sativa leaves with a solvent; the volume ratio of the solvent is 10:1-4 of water and ethanol;
The content of the manganese chloride supermolecule of the ethyl diiminomethyl guaiacol is 0.1 to 1 part by weight, the content of the ergothioneine is 0.1 to 1 part by weight, the content of the palmitoyl tetrapeptide-7 is 0.1 to 1 part by weight, and the content of the extract combination is 1 to 10 parts by weight, relative to 100 parts by weight of the mannitol;
The ethyl bis iminomethyl guaiacol manganese chloride supermolecule is prepared by a method comprising the following steps:
Performing first stirring on the cyclodextrin derivative and the ethyl bis (iminomethyl) guaiacol manganese chloride, and then performing first spray drying to obtain the ethyl bis (iminomethyl) guaiacol manganese chloride supermolecule;
The cyclodextrin derivative is at least one selected from hydroxypropyl beta cyclodextrin and hydroxyethyl beta cyclodextrin.
2. The composition of claim 1, wherein the first agitating conditions comprise: the time is 1-3h, and the temperature is 70-90 ℃;
And/or, the conditions of the first spray drying include: the temperature is 110-130 ℃, and the sample injection speed is 10-20mL/min.
3. The composition of claim 1, wherein the cyclodextrin derivative is present in an amount by weight of 1:0.1-0.5.
4. A method for preparing freeze-dried powder with anti-aging and repairing effects, which is characterized in that the method is prepared by using the components in the freeze-dried powder composition as claimed in any one of claims 1 to 3, and comprises the following steps:
(1) Preparation of extract combinations: the weight ratio of the dosage is 1: extracting Lespedeza capitata of 0.5-1 with solvent to obtain the extract combination;
(2) Mixing ethyl diiminomethyl guaiacol manganese chloride supermolecule, ergothioneine, palmitoyl tetrapeptide-7, mannitol and the extract combination in the presence of water to obtain a material I;
(3) And freeze-drying the material I to obtain the freeze-dried powder.
5. The production method according to claim 4, wherein, in the step (1), the conditions of the solvent extraction include: the temperature is 50-80deg.C, and the time is 20-40min.
6. The production method according to claim 4 or 5, wherein, in step (3), the conditions of lyophilization include: the temperature is between-50 ℃ and-30 ℃ and the time is between 2 and 5 hours.
7. Lyophilized powder having anti-aging effect obtained by the preparation method of any one of claims 4 to 6.
8. Use of the lyophilized powder of claim 7 in a skin cosmetic.
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| CN110897923A (en) * | 2019-11-28 | 2020-03-24 | 修之妍(厦门)生物科技有限公司 | Cosmetic auxiliary material with synergistic antioxidation effect and cosmetic |
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