CN117547486A - Protection method of oil-soluble active ingredient - Google Patents
Protection method of oil-soluble active ingredient Download PDFInfo
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- CN117547486A CN117547486A CN202410038599.1A CN202410038599A CN117547486A CN 117547486 A CN117547486 A CN 117547486A CN 202410038599 A CN202410038599 A CN 202410038599A CN 117547486 A CN117547486 A CN 117547486A
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- Prior art keywords
- oil
- soluble active
- active ingredient
- stirring
- homogenizing
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- 239000004480 active ingredient Substances 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 65
- 238000003756 stirring Methods 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 claims abstract description 17
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims abstract description 17
- 229940068968 polysorbate 80 Drugs 0.000 claims abstract description 17
- 229920000053 polysorbate 80 Polymers 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 15
- 239000002562 thickening agent Substances 0.000 claims abstract description 14
- 239000004519 grease Substances 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 230000008961 swelling Effects 0.000 claims abstract description 6
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 5
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 24
- LADGBHLMCUINGV-UHFFFAOYSA-N tricaprin Chemical compound CCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCC)COC(=O)CCCCCCCCC LADGBHLMCUINGV-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 230000002633 protecting effect Effects 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 12
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 12
- -1 polydimethylsiloxane Polymers 0.000 claims description 12
- 229940090934 diphenylsiloxy phenyl trimethicone Drugs 0.000 claims description 11
- VYGQUTWHTHXGQB-FFHKNEKCSA-N Retinol Palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C VYGQUTWHTHXGQB-FFHKNEKCSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 229920002125 Sokalan® Polymers 0.000 claims description 5
- 230000001276 controlling effect Effects 0.000 claims description 5
- 239000004744 fabric Substances 0.000 claims description 5
- 239000011236 particulate material Substances 0.000 claims description 5
- 229940108325 retinyl palmitate Drugs 0.000 claims description 5
- 235000019172 retinyl palmitate Nutrition 0.000 claims description 5
- 239000011769 retinyl palmitate Substances 0.000 claims description 5
- VNXWANZMRATDQM-UHFFFAOYSA-N 2-(2-phenylethyl)benzene-1,3-diol Chemical compound OC1=CC=CC(O)=C1CCC1=CC=CC=C1 VNXWANZMRATDQM-UHFFFAOYSA-N 0.000 claims description 3
- CSHZYWUPJWVTMQ-UHFFFAOYSA-N 4-n-Butylresorcinol Chemical compound CCCCC1=CC=C(O)C=C1O CSHZYWUPJWVTMQ-UHFFFAOYSA-N 0.000 claims description 3
- 241000130781 Arnebia Species 0.000 claims description 3
- 238000007792 addition Methods 0.000 claims description 3
- 239000004475 Arginine Substances 0.000 claims description 2
- ACTIUHUUMQJHFO-UHFFFAOYSA-N Coenzym Q10 Natural products COC1=C(OC)C(=O)C(CC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UHFFFAOYSA-N 0.000 claims description 2
- ODKSFYDXXFIFQN-BYPYZUCNSA-P L-argininium(2+) Chemical compound NC(=[NH2+])NCCC[C@H]([NH3+])C(O)=O ODKSFYDXXFIFQN-BYPYZUCNSA-P 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 claims description 2
- ACTIUHUUMQJHFO-UPTCCGCDSA-N coenzyme Q10 Chemical compound COC1=C(OC)C(=O)C(C\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UPTCCGCDSA-N 0.000 claims description 2
- 235000017471 coenzyme Q10 Nutrition 0.000 claims description 2
- NPCOQXAVBJJZBQ-UHFFFAOYSA-N reduced coenzyme Q9 Natural products COC1=C(O)C(C)=C(CC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)C)C(O)=C1OC NPCOQXAVBJJZBQ-UHFFFAOYSA-N 0.000 claims description 2
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 2
- 229960000281 trometamol Drugs 0.000 claims description 2
- 229940035936 ubiquinone Drugs 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 239000002537 cosmetic Substances 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 29
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 210000003491 skin Anatomy 0.000 description 7
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 description 6
- 229960002446 octanoic acid Drugs 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 4
- 229960001631 carbomer Drugs 0.000 description 4
- 229940075509 carbomer 1342 Drugs 0.000 description 3
- 229940085237 carbomer-980 Drugs 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 210000003205 muscle Anatomy 0.000 description 3
- 235000014593 oils and fats Nutrition 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 2
- SNPLKNRPJHDVJA-ZETCQYMHSA-N D-panthenol Chemical group OCC(C)(C)[C@@H](O)C(=O)NCCCO SNPLKNRPJHDVJA-ZETCQYMHSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 125000006267 biphenyl group Chemical group 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229940101267 panthenol Drugs 0.000 description 1
- 235000020957 pantothenol Nutrition 0.000 description 1
- 239000011619 pantothenol Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 210000004927 skin cell Anatomy 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 210000000434 stratum corneum Anatomy 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
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- 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
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
-
- 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
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
-
- 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
- A61K8/31—Hydrocarbons
-
- 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
- A61K8/347—Phenols
-
- 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
- A61K8/35—Ketones, e.g. benzophenone
- A61K8/355—Quinones
-
- 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
- A61K8/37—Esters of carboxylic acids
- A61K8/375—Esters of carboxylic acids the alcohol moiety 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
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/41—Amines
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- 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
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated 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
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4993—Derivatives containing from 2 to 10 oxyalkylene groups
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- 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
- A61K8/585—Organosilicon compounds
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- 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
- A61K8/67—Vitamins
- A61K8/671—Vitamin A; Derivatives thereof, e.g. ester of vitamin A acid, ester of retinol, retinol, retinal
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- A—HUMAN NECESSITIES
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- 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
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- A61K8/8147—Homopolymers or copolymers of acids; Metal or ammonium salts thereof, e.g. crotonic acid, (meth)acrylic acid; Compositions of derivatives of such polymers
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- 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
- A61K8/89—Polysiloxanes
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
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- 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
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- 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
- A61K2800/10—General cosmetic use
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- 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
- A61K2800/48—Thickener, Thickening system
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Emergency Medicine (AREA)
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
- Dermatology (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a protection method of oil-soluble active ingredients, which comprises the following steps: (1) Adding a thickening agent into deionized water, completely swelling, heating, and starting to homogenize; (2) Adding a pH regulator and polysorbate-80 to obtain a water phase; (3) Uniformly mixing grease, oil-soluble active ingredients, an emulsifying agent and a color regulator in a reaction kettle to prepare an oil phase; (4) Heating, adding water phase while stirring the oil phase, stirring until the particles are dispersed uniformly, removing ethanol by rotary evaporation, homogenizing, and filtering to obtain the protected active ingredient. The invention ensures that all components are tightly adhered and fully permeated through the treatment of the added components and the simple preparation process, wherein the use of polysorbate-80 and ethanol solvent can improve the compatibility between the oil-soluble active component and the water agent and other components, wrap the oil-soluble active component to form a stable system which is not easy to influence the activity, improve the activity effect of the oil-soluble active component absorbed by skin and improve the application of the oil-soluble active component in cosmetics.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to a protection method of oil-soluble active ingredients.
Background
With the expansion of the application range of cosmetics and the improvement of skin care consciousness, the demand for functional cosmetics is increasing. The existing cosmetics sold in the market mostly achieve the effect of various skin care by adding components with different functions, wherein the addition of natural active components and derivatives thereof is favored, compared with water-soluble active components, the oil-soluble active components have stronger and longer efficacy, however, the skin is used as a natural barrier for resisting the influence of external environment, the compact stratum corneum of the skin can play an effective role in protecting, on the other hand, sensitive muscles are many, so that the cosmetics with more components and thick texture are also blocked to a certain extent in absorption, only a small amount of oil-soluble active components can enter pores and be absorbed by skin cells, and the cosmetics are not friendly to sensitive muscles and are easy to aggravate the burden of the sensitive muscles.
In addition, the oil-soluble active ingredients have limited dissolving capacity in the water aqua, poor compatibility with the water aqua, and many oil-soluble active ingredients are easily affected by factors such as heat, solubility, pH and the like when being prepared or used, for example, the oil-soluble active ingredients are easy to deactivate when being heated at high temperature and easy to precipitate when being treated at low temperature, so that the utilization rate is reduced and the activity is precipitated, therefore, the loss of the oil-soluble active ingredients is possibly reduced in the early stage of preparation, and a stable system with high active transdermal absorptivity and mild skin is formed, which is a problem to be solved at present.
Disclosure of Invention
In order to overcome the technical problems in the prior art, the invention firstly provides a protection method for oil-soluble active ingredients, and the treatment of the added components and the simple preparation process enable the components to be closely adhered and fully permeated to form a stable system with the active ingredients not easy to separate out, so that the active effect of the oil-soluble active ingredients is improved, and the application of the oil-soluble active ingredients in cosmetics is effectively protected.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a protection method of oil-soluble active ingredients, which comprises the following steps:
(1) Adding the thickener into deionized water to completely swell, heating, starting homogenizing, and stopping homogenizing when no particles exist;
(2) Adding a pH regulator and polysorbate-80 to obtain a water phase;
(3) Uniformly mixing grease, oil-soluble active ingredients, an emulsifying agent and a color regulator in a reaction kettle to prepare an oil phase;
(4) Heating, adding water phase while stirring the oil phase, stirring until the particles are dispersed uniformly, removing ethanol by rotary evaporation, homogenizing, and filtering to obtain the protected active ingredient.
Preferably, the protection method comprises the steps of:
(1) Adding thickener into deionized water, swelling completely, heating to 70-75deg.C, setting homogenizing pressure of high pressure homogenizer to 900-1100bar and homogenizing speed to 4500-6500rmp, starting homogenizing, and stopping homogenizing when no particles exist;
(2) Adding pH regulator and polysorbate-80, and regulating pH to 5-6 to obtain water phase;
(3) Uniformly mixing grease, oil-soluble active ingredients, an emulsifying agent and a color regulator in a reaction kettle to prepare an oil phase;
(4) Heating to 60-65deg.C, controlling stirring speed to 300-400rmp, adding water phase while stirring oil phase, stirring to uniformly disperse particles, removing ethanol by rotary evaporation at 50-60deg.C, homogenizing under high pressure of 700-800bar at 3800-4200rmp for 8-12min for three times, and filtering with 200 mesh filter cloth to obtain uniform particulate material as the protected active ingredient.
Preferably, the oil-soluble active ingredient accounts for 0.1-1% of the total reaction system, wherein the oil-soluble active ingredient is selected from one or more of 4-butylresorcinol, phenethyl resorcinol, retinol palmitate, arnebia oil, guaazulene and ubiquinone.
Preferably, the thickener comprises various types of carbomer, accounting for 0.03-0.1% of the total reaction system; the pH regulator mainly refers to an alkaline pH regulator, and comprises any one of sodium hydroxide, arginine, triethanolamine, potassium hydroxide and tromethamine, and accounts for 0.02-0.08% of the total reaction system.
Preferably, the polysorbate-80 accounts for 0.3-1.1% of the total reaction system; the emulsifier accounts for 2.5-5% of the total reaction system; the color regulator accounts for 0.00001-1% of the total reaction system.
Preferably, the grease comprises caprylic/capric triglyceride, polydimethylsiloxane, diphenylsiloxyphenyl trimethicone and diphenylpolydimethylsiloxane, and accounts for 13-20% of the total reaction system.
Preferably, the preparation method of the oil phase comprises the following steps:
slowly adding 2-3 parts of caprylic/capric triglyceride into a reaction kettle, adding absolute ethyl alcohol with the volume being 6-8 times of that of the caprylic/capric triglyceride for mixing, stirring uniformly, adding and stirring twice, sequentially adding an oil-soluble active ingredient, an emulsifying agent and a color regulator according to parts by weight, mixing uniformly, and stirring at the temperature of 60-70 ℃ and the rotating speed of 100-300rmp until no bubbles exist, thus obtaining the oil phase.
Preferably, the reaction condition of the reaction kettle is that the temperature is 95-105 ℃ and the pressure is 0.3-0.5KPa under the nitrogen environment.
Preferably, the first of the two feeds is 0.8-1.6 parts of polydimethylsiloxane and is stirred for 60-90min at 82-92 ℃ and a rotational speed of 700-900 rmp.
Preferably, the second of the two feeds is to add 0.3 to 0.8 part of diphenylsiloxyphenyl trimethicone and 0.25 to 0.45 part of diphenylpolydimethylsiloxane, and stir at 72 to 78 ℃ and 400 to 600rmp of rotation speed for 45 to 55 minutes.
The invention has the beneficial effects that:
the invention provides a protection method of oil-soluble active ingredients, which is characterized in that water phase and oil phase are respectively prepared, and finally the water phase and the oil phase are mutually melted, so that the process is simple and easy to operate.
The grease is formed by processing caprylic/capric triglyceride, polydimethylsiloxane, diphenyl siloxyphenyl trimethyl siloxane and diphenyl dimethyl polysiloxane through a specific process, coupling is formed in the grease, the grease is more compact and uniform, and components such as an oil-soluble active component, a thickening agent and an emulsifying agent are added according to a specific proportion, so that the oil-soluble active component can be better permeated and coated; the polysorbate-80 is added into the water phase, so that the compatibility between the water phase and the oil phase can be improved, and all the components are compatible and synergistic, so that the whole system is more stable and uniform, the active effect of the oil-soluble active ingredient is further improved, and the application of the oil-soluble active ingredient in cosmetics is effectively protected.
The protection method can effectively help the active ingredients to slowly release into the skin, reduce the sensitivity rate of the skin and improve the activity utilization rate of the raw material ingredients; on the other hand, the raw materials are regulated through the mutual matching of the components, so that the appearance and the state of the raw materials are more uniform and attractive.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below in connection with specific embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The protection method of the oil-soluble active ingredient comprises the following steps:
(1) Adding a thickening agent into deionized water, fully swelling, heating to 70 ℃, setting the homogenizing pressure of a high-pressure homogenizer to 900bar, the homogenizing speed to 4500rmp, starting homogenizing, and stopping homogenizing until no particles exist;
(2) Adding pH regulator and polysorbate-80, and regulating pH to 5 to obtain water phase;
(3) Uniformly mixing grease, oil-soluble active ingredients, an emulsifying agent and a color regulator in a reaction kettle to prepare an oil phase;
(4) Heating to 60deg.C, controlling stirring speed to 300rmp, adding water phase into oil phase under stirring, stirring to disperse the particles uniformly, steaming at 50deg.C to remove ethanol, homogenizing under pressure of 700bar, homogenizing speed of 3800rmp, homogenizing for 8min, homogenizing for three times, and filtering with 200 mesh filter cloth to obtain uniform particulate material as the protected active ingredient.
The oil-soluble active ingredient of this example is retinol palmitate, accounting for 0.3% of the total reaction system.
The thickener of this example included carbomer 980, carbomer 981 and carbomer 1342, accounting for 0.03% of the total reaction system; the pH regulator in this example was sodium hydroxide, accounting for 0.02% of the total reaction system.
Polysorbate-80 in this example was 0.3% of the total reaction system; the emulsifier of this example was 2.5% of the total reaction system; the color modifier of this example represents 0.00001% of the total reaction system.
The oils and fats of this example include caprylic/capric triglyceride, polydimethylsiloxane, diphenylsiloxyphenyl trimethicone, and diphenylpolydimethylsiloxane, accounting for 13% of the total reaction system.
The preparation method of the oil phase in the embodiment comprises the following steps:
slowly adding 2 parts of caprylic acid/capric acid triglyceride into a reaction kettle, adding absolute ethyl alcohol with the volume of 6 times of that of the caprylic acid/capric acid triglyceride for mixing, stirring uniformly, adding and stirring twice, sequentially adding an oil-soluble active ingredient, an emulsifying agent and a color regulator according to parts by weight, stirring uniformly at the temperature of 60 ℃ and the rotating speed of 100rmp until no bubbles exist, and obtaining the oil phase.
The reaction conditions of the reaction kettle of the embodiment are that the temperature is 95 ℃ and the pressure is 0.3KPa under the nitrogen environment.
The first of the two feeds in this example was 0.8 part polydimethylsiloxane and stirred at 82℃and 700rmp for 60min.
The second of the two feeds of this example was 0.3 part diphenylsiloxyphenyl trimethicone and 0.25 part diphenylpolydimethylsiloxane and stirred at 72℃and 400rmp for 45min.
Example 2
The protection method of the oil-soluble active ingredient comprises the following steps:
(1) Adding the thickener into deionized water, swelling completely, heating to 75deg.C, setting homogenizing pressure of 1100bar and homogenizing speed of 6500rmp, starting homogenizing, and stopping homogenizing when no particles exist;
(2) Adding pH regulator and polysorbate-80, and regulating pH to 6 to obtain water phase;
(3) Uniformly mixing grease, oil-soluble active ingredients, an emulsifying agent and a color regulator in a reaction kettle to prepare an oil phase;
(4) Heating to 65deg.C, controlling stirring speed to 400rmp, adding water phase while stirring oil phase, stirring to disperse the particles uniformly, removing ethanol by rotary steaming at 60deg.C, homogenizing under 800bar at 4200rmp for 12min for three times, and filtering with 200 mesh filter cloth to obtain uniform particulate material as the protected active ingredient.
The oil-soluble active ingredient of this example is retinol palmitate, accounting for 0.3% of the total reaction system.
The thickener of this example included carbomer 980, carbomer 981 and carbomer 1342, accounting for 0.1% of the total reaction system; the pH regulator in this example was sodium hydroxide, accounting for 0.08% of the total reaction system.
Polysorbate-80 in this example was 1.1% of the total reaction system; the emulsifier of this example is 5% of the total reaction system; the color modifier of this example represents 1% of the total reaction system.
The oils and fats of this example include caprylic/capric triglyceride, polydimethylsiloxane, diphenylsiloxyphenyl trimethicone, and diphenylpolydimethylsiloxane, accounting for 20% of the total reaction system.
The preparation method of the oil phase in the embodiment comprises the following steps:
slowly adding 3 parts of caprylic acid/capric acid triglyceride into a reaction kettle, adding absolute ethyl alcohol with the volume being 8 times of that of the caprylic acid/capric acid triglyceride for mixing, stirring uniformly, adding and stirring twice, sequentially adding an oil-soluble active ingredient, an emulsifying agent and a color regulator according to parts by weight, stirring uniformly at the temperature of 70 ℃ and the rotating speed of 300rmp until no bubbles exist, and obtaining the oil phase.
The reaction conditions of the reaction kettle of the embodiment are that the temperature is 105 ℃ and the pressure is 0.5KPa under the nitrogen environment.
The first of the two feeds in this example was 1.6 parts of polydimethylsiloxane and stirred for 90min at 92℃and 900 rmp.
The second of the two feeds of this example was 0.8 part diphenylsiloxyphenyl trimethicone and 0.45 part diphenylpolydimethylsiloxane and stirred at 78℃and 600rmp for 55min.
Example 3
The protection method of the oil-soluble active ingredient comprises the following steps:
(1) Adding the thickener into deionized water, swelling completely, heating to 70-75deg.C, setting homogenizing pressure of high pressure homogenizer to 1000bar and homogenizing speed to 5500rmp, starting homogenizing, and stopping homogenizing when no particles exist;
(2) Adding pH regulator and polysorbate-80, and regulating pH to 5.5 to obtain water phase;
(3) Uniformly mixing grease, oil-soluble active ingredients, an emulsifying agent and a color regulator in a reaction kettle to prepare an oil phase;
(4) Heating to 62deg.C, controlling stirring speed to 350rmp, adding water phase while stirring oil phase, stirring to disperse the particles uniformly, removing ethanol by rotary steaming at 55deg.C, homogenizing under 750bar, 4000rmp, homogenizing for 10min for three times, and filtering with 200 mesh filter cloth to obtain uniform particulate material as the protected active ingredient.
The oil-soluble active ingredient of this example is retinol palmitate, accounting for 0.3% of the total reaction system.
The thickener of this example included carbomer 980, carbomer 981 and carbomer 1342, accounting for 0.06% of the total reaction system; the pH regulator in this example was sodium hydroxide, accounting for 0.05% of the total reaction system.
Polysorbate-80 in this example was 0.7% of the total reaction system; the emulsifier of this example represents 3.75% of the total reaction system; the color modifier of this example represents 0.5% of the total reaction system.
The oils and fats of this example include caprylic/capric triglyceride, polydimethylsiloxane, diphenylsiloxyphenyl trimethicone, and diphenylpolydimethylsiloxane, accounting for 16.5% of the total reaction system.
The preparation method of the oil phase in the embodiment comprises the following steps:
slowly adding 2.5 parts of caprylic acid/capric acid triglyceride into a reaction kettle, adding absolute ethyl alcohol with the volume being 7 times of that of the caprylic acid/capric acid triglyceride for mixing, stirring uniformly, adding and stirring twice, sequentially adding an oil-soluble active ingredient, an emulsifying agent and a color regulator according to parts by weight, mixing uniformly, and stirring at the temperature of 65 ℃ and the rotating speed of 200rmp until no bubbles exist, thus obtaining the oil phase.
The reaction conditions of the reaction kettle of the embodiment are that the temperature is 100 ℃ and the pressure is 0.4KPa under the nitrogen environment.
The first of the two feeds in this example was 1.2 parts of polydimethylsiloxane and stirred at 87℃and 800rmp for 75min.
The second of the two feeds of this example was 0.55 part diphenylsiloxyphenyl trimethicone and 0.35 part diphenylpolydimethylsiloxane and stirred at 75℃and 400-600rmp for 50min.
Example 4
In the process of example 3, the oil-soluble active ingredients were replaced with phenethyl resorcinol and 4-butyl resorcinol, accounting for 1% of the total reaction system.
Example 5
In the process of example 3, the oil-soluble active ingredient was replaced with arnebia oil, accounting for 0.8% of the total reaction system.
Example 6
In the process of example 3, the oil-soluble active ingredient was replaced with guaazulene, accounting for 0.6% of the total reaction system.
Example 7
In the process of example 3, the oil-soluble active ingredient was replaced with panthenol in an amount of 0.75% of the total reaction system.
Comparative example 1.
The difference from example 3 is that the fat is only caprylic/capric triglyceride.
Comparative example 2.
Unlike example 3, the oil phase was prepared by the following method:
2.5 parts of caprylic/capric triglyceride, 1.2 parts of polydimethylsiloxane, 0.55 part of diphenylsiloxyphenyl trimethicone and 0.35 part of diphenylpolydimethylsiloxane are sequentially added into a reaction kettle according to parts by weight, and after being uniformly mixed, the oil-soluble active ingredient, the emulsifier and the color regulator are stirred at the temperature of 65 ℃ and the rotating speed of 200rmp until no bubbles exist, so that the oil phase is obtained.
The reaction conditions of the reaction kettle of the comparative example are that the temperature is 100 ℃ and the pressure is 0.4KPa under the nitrogen environment.
Comparative example 3.
Unlike example 3, polysorbate-80 was not added.
The stability test was conducted by taking the essence emulsions prepared in examples 1 to 3 and comparative examples 1 to 3, each of which was sampled 5 groups of 50g each, and after storing for 15d and 30d in a low temperature (-10 ℃) environment, a room temperature and high temperature (50 ℃) environment, and a high and low temperature alternating (-10 to 50 ℃) environment, the appearance and feel of the products were compared, and the test results were shown in table 1 below.
As can be seen from Table 1, the products prepared by the protection methods of examples 1-3 of the present invention can still maintain good stability after periodic testing in low temperature, high temperature and high and low temperature alternate environments, have good experience feeling in use, are easy to melt and smear, and can still maintain stability and use feeling of the products by replacing the oil-soluble active ingredients in the products according to examples 4-7 of the present invention, so that the protection methods can improve stability and compatibility of each oil-soluble active ingredient in the whole system, and effectively protect application of the oil-soluble active ingredients in cosmetics.
As is clear from comparative examples 3 and 1 and 2, only one component is added as the oil, or the compatibility of components such as oil phase water agent is blocked by simple mutual matching and mixing of various components, so that the ideal effect of protecting oil-soluble active components cannot be achieved, and the oil prepared by the protecting method can exist more stably and uniformly in the whole system, has better protecting effect on the oil-soluble active components, and better plays the role of the oil-soluble active components.
As can be seen from comparative example 3 and comparative example 3, the use of polysorbate-80 can better improve the compatibility between the oil phase and the water phase, and the prepared product has smaller influence on the low-temperature, high-temperature and high-low-temperature alternate environment and better use effect.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A method for protecting an oil-soluble active ingredient, the method comprising the steps of:
adding the thickener into deionized water to completely swell, heating, starting homogenizing, and stopping homogenizing when no particles exist;
adding a pH regulator and polysorbate-80 to obtain a water phase;
uniformly mixing grease, oil-soluble active ingredients, an emulsifying agent and a color regulator in a reaction kettle to prepare an oil phase;
heating, adding water phase while stirring the oil phase, stirring until the particles are dispersed uniformly, removing ethanol by rotary evaporation, homogenizing, and filtering to obtain the protected active ingredient.
2. A method of protecting an oil-soluble active ingredient according to claim 1, comprising the steps of:
(1) Adding thickener into deionized water, swelling completely, heating to 70-75deg.C, setting homogenizing pressure of high pressure homogenizer to 900-1100bar and homogenizing speed to 4500-6500rmp, starting homogenizing, and stopping homogenizing when no particles exist;
(2) Adding pH regulator and polysorbate-80, and regulating pH to 5-6 to obtain water phase;
(3) Uniformly mixing grease, oil-soluble active ingredients, an emulsifying agent and a color regulator in a reaction kettle to prepare an oil phase;
(4) Heating to 60-65deg.C, controlling stirring speed to 300-400rmp, adding water phase while stirring oil phase, stirring to uniformly disperse particles, removing ethanol by rotary evaporation at 50-60deg.C, homogenizing under high pressure of 700-800bar at 3800-4200rmp for 8-12min for three times, and filtering with 200 mesh filter cloth to obtain uniform particulate material as the protected active ingredient.
3. The method for protecting an oil-soluble active ingredient according to claim 1, wherein the oil-soluble active ingredient is 0.1-1% of the total reaction system, wherein the oil-soluble active ingredient is one or more selected from 4-butylresorcinol, phenethyl resorcinol, retinol palmitate, arnebia oil, guaia and ubiquinone.
4. The method for protecting an oil-soluble active ingredient according to claim 1, wherein the thickener comprises various types of carbomers accounting for 0.03-0.1% of the total reaction system; the pH regulator mainly refers to an alkaline pH regulator, and comprises any one of sodium hydroxide, arginine, triethanolamine, potassium hydroxide and tromethamine, and accounts for 0.02-0.08% of the total reaction system.
5. The method for protecting an oil-soluble active ingredient according to claim 1, wherein polysorbate-80 is 0.3 to 1.1% of the total reaction system; the emulsifier accounts for 2.5-5% of the total reaction system; the color regulator accounts for 0.00001-1% of the total reaction system.
6. The method for protecting an oil-soluble active ingredient according to claim 1, wherein the oil comprises caprylic/capric triglyceride, polydimethylsiloxane, diphenylsiloxyphenyl trimethicone, and diphenylpolydimethylsiloxane, and is 13-20% of the total reaction system.
7. The method for protecting an oil-soluble active ingredient according to claim 1, wherein the oil phase is prepared by the following steps:
slowly adding 2-3 parts of caprylic/capric triglyceride into a reaction kettle, adding absolute ethyl alcohol with the volume being 6-8 times of that of the caprylic/capric triglyceride for mixing, stirring uniformly, adding and stirring twice, sequentially adding an oil-soluble active ingredient, an emulsifying agent and a color regulator according to parts by weight, mixing uniformly, and stirring at the temperature of 60-70 ℃ and the rotating speed of 100-300rmp until no bubbles exist, thus obtaining the oil phase.
8. The method for protecting an oil-soluble active ingredient according to claim 7, wherein the reaction condition of the reaction kettle is that the temperature is 95-105 ℃ and the pressure is 0.3-0.5KPa under the nitrogen environment.
9. The method for protecting an oil-soluble active ingredient according to claim 7, wherein the first charge of the two charges is 0.8 to 1.6 parts of polydimethylsiloxane, and the mixture is stirred for 60 to 90 minutes at a temperature of 82 to 92 ℃ and a rotational speed of 700 to 900 rmp.
10. The method for protecting an oil-soluble active ingredient according to claim 7, wherein the second addition of the two additions is to add 0.3 to 0.8 part of diphenylsiloxyphenyl trimethicone and 0.25 to 0.45 part of diphenylpolydimethylsiloxane, and stir at 72 to 78 ℃ and 400 to 600rmp for 45 to 55 minutes.
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