CN112516014A - Apocynum venetum extract, preparation method thereof, anti-ultraviolet, anti-oxidation and whitening cosmetic and preparation method thereof - Google Patents
Apocynum venetum extract, preparation method thereof, anti-ultraviolet, anti-oxidation and whitening cosmetic and preparation method thereof Download PDFInfo
- Publication number
- CN112516014A CN112516014A CN202110045678.1A CN202110045678A CN112516014A CN 112516014 A CN112516014 A CN 112516014A CN 202110045678 A CN202110045678 A CN 202110045678A CN 112516014 A CN112516014 A CN 112516014A
- Authority
- CN
- China
- Prior art keywords
- apocynum venetum
- polysaccharide
- ultraviolet
- extract
- preparation
- 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.)
- Granted
Links
Images
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
- A61K8/92—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
- A61K8/29—Titanium; Compounds 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
- A61K8/31—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
-
- 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
- A61K8/342—Alcohols having more than seven atoms in an unbroken chain
-
- 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
- A61K8/361—Carboxylic acids having more than seven carbon atoms in an unbroken chain; 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
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/37—Esters of carboxylic acids
-
- 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
-
- 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
- A61K8/67—Vitamins
- A61K8/678—Tocopherol, i.e. vitamin E
-
- 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
-
- 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
- A61K8/89—Polysiloxanes
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning 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
- A61Q19/02—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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
-
- 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
- A61K2800/74—Biological properties of particular ingredients
- A61K2800/78—Enzyme modulators, e.g. Enzyme agonists
- A61K2800/782—Enzyme inhibitors; Enzyme antagonists
-
- 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
- A61K2800/82—Preparation or application process involves sonication or ultrasonication
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Animal Behavior & Ethology (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Chemical & Material Sciences (AREA)
- Emergency Medicine (AREA)
- Engineering & Computer Science (AREA)
- Dermatology (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Wood Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Materials Engineering (AREA)
- Sustainable Development (AREA)
- Inorganic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Cosmetics (AREA)
Abstract
The invention belongs to the technical field of cosmetics, and particularly relates to an apocynum venetum extract and a preparation method thereof, and an anti-ultraviolet anti-oxidation whitening cosmetic and a preparation method thereof. The invention provides a apocynum venetum extract, which comprises the effective components of apocynum venetum essential oil and apocynum venetum polysaccharide. The apocynum venetum polysaccharide has excellent antioxidant and anti-ultraviolet radiation effects besides the common water-locking and moisturizing effects, and can protect the skin and isolate external stimulation, inflammation and ultraviolet pollution; the apocynum venetum essential oil has excellent tyrosinase activity inhibition effect, can inhibit the generation of melanin, and has the whitening effect. The apocynum venetum extract is applied to cosmetics, and under the combined action of the apocynum venetum extract and other components, the cosmetics have the effects of resisting ultraviolet radiation, resisting oxidation and whitening.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to an apocynum venetum extract and a preparation method thereof, and an anti-ultraviolet anti-oxidation whitening cosmetic and a preparation method thereof.
Background
In areas with inflammation and strong sunshine, the sunscreen cosmetics are indispensable products for consumers. The skin is the largest organ of the human body and is the first line of defense of the human body, the skin exposed to the outside in the human body, such as the face, the neck, the upper and lower limbs and other parts, is extremely easy to be damaged by ultraviolet rays, and the sunscreen cosmetics can protect the skin of the exposed part of the human body. In China, sunscreen cosmetics belong to special-purpose cosmetics, and refer to cosmetics capable of preventing or reducing skin damage caused by ultraviolet radiation.
Ultraviolet rays which damage human skin are mainly divided into two wave bands of UVB (290-320 nm) and UVA (320-400 nm) according to different wavelengths, wherein the UVB mainly acts on the epidermis of the skin, the UVA mainly acts on the dermis, and the depth of the UVB can reach the middle of the dermis. The ultraviolet rays are the first killer of the skin, can cause oxidative damage to the skin, can induce the generation of various Reactive Oxygen Species (ROS), and the ROS can trigger various physiological and biochemical processes, so that excessive ROS generated in cells can cause damage to biomacromolecules in the cells if not cleared in time, thereby causing the redox state of the cells to be changed, inducing apoptosis and causing acute and chronic damage to the skin.
Sunscreen cosmetics mainly rely on sunscreen agents to protect against ultraviolet rays, and are classified into physical sunscreen agents and chemical sunscreen agents. Physical sunscreens do not absorb ultraviolet light, primarily function to reflect and scatter ultraviolet light, also known as inorganic sunscreens, such as titanium dioxide, zinc oxide, kaolin, talc, iron oxide, and the like; the chemical sunscreen agent mainly has the function of absorbing ultraviolet rays, and common chemical sunscreen agents comprise benzophenone, ethylhexyl salicylate and the like; however, chemical sunscreens are somewhat irritating to the skin because the molecules of the chemical sunscreen are absorbed by the skin and the process of absorbing ultraviolet light occurs inside the skin. In addition to these two traditional sunscreens, people focus on finding new bioactive substances capable of resisting ultraviolet radiation, which are safe and efficient, from animals and plants as novel sunscreens, and the research focus in the field of current sunscreen cosmetics is also hot.
Apocynum venetum L is an erect shrub of Apocynaceae, and is mainly distributed on saline-alkali wastelands, desert edges, river banks and gobi barren beaches in provinces such as Xinjiang, Qinghai, Gansu and inner Mongolia in China. Besides the fibers in the stems of the apocynum venetum can be used as high-grade textile raw materials, the apocynum venetum leaves are rich in active compounds such as flavone, organic acid, polysaccharide and the like, and can be used for developing and preparing raw materials of plant-derived cosmetics. However, the apocynum venetum extract prepared by the prior art has single effective component and single skin care effect.
Disclosure of Invention
The invention provides an apocynum venetum extract which comprises apocynum venetum essential oil and apocynum venetum polysaccharide, and can effectively play roles in resisting ultraviolet radiation, resisting oxidation and whitening when being applied to cosmetics.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a apocynum venetum extract, which comprises the effective components of apocynum venetum essential oil and apocynum venetum polysaccharide.
The invention also provides a preparation method of the apocynum venetum extract, which comprises the following steps:
carrying out ultrasonic extraction on the dogbane leaves to obtain a primary extract;
distilling the primary extract to obtain apocynum venetum essential oil and an extracting solution;
and filtering and extracting the extracting solution with alcohol to obtain the apocynum venetum polysaccharide.
Preferably, the power of ultrasonic extraction is 200-300W, the time is 60-120 min, and the temperature is 50-70 ℃.
Preferably, the distillation is steam distillation, and the distillation time is 2-4 h.
Preferably, the refining of the apocynum venetum polysaccharide after the apocynum venetum polysaccharide is obtained comprises enzyme hydrolysis and impurity removal.
Preferably, the impurity removal reagent is chloroform and n-butyl alcohol, and the mass ratio of the chloroform to the n-butyl alcohol is 3-6: 1.
The invention also provides the application of the apocynum venetum extract in the ultraviolet radiation resistant, antioxidant and whitening cosmetics.
The invention also provides an anti-ultraviolet antioxidant whitening cosmetic which comprises the following components in percentage by mass: 2-12% of apocynum venetum extract, 3-8% of stearic acid, 1.5-4% of octadecanol, 1-3% of isopropyl palmitate, 3-8% of vaseline, 2-6% of white oil, 3-8% of silicone oil, 0.5-1.5% of vitamin E, 1-3% of emulsifier, 2-5% of propylene glycol, 2-5% of nano titanium dioxide, 0.5-1.5% of triethanolamine, 0.3-1.0% of phenoxyethanol and the balance of water;
the apocynum venetum extract is the apocynum venetum extract in the technical scheme.
Preferably, the content of the apocynum venetum essential oil in the anti-ultraviolet, antioxidant and whitening cosmetic is 0.5-3%, and the content of the apocynum venetum polysaccharide is 1.5-9%.
The invention also provides a preparation method of the ultraviolet-resistant sunscreen whitening cosmetic, which comprises the following steps:
mixing stearic acid, octadecanol, isopropyl palmitate, vaseline, white oil, silicone oil, vitamin E and an emulsifier to obtain an oil phase system;
dispersing propylene glycol, nano titanium dioxide, apocynum venetum polysaccharide and triethanolamine in water to obtain a water phase system;
and mixing the oil phase system and the water phase system with the apocynum venetum essential oil and the phenoxyethanol to obtain the anti-ultraviolet anti-oxidation whitening cosmetic.
The invention provides an apocynum venetum extract, which comprises apocynum venetum essential oil and apocynum venetum polysaccharide. The apocynum venetum essential oil has excellent tyrosinase activity inhibition, can inhibit the generation of melanin, and has the whitening effect; the apocynum venetum polysaccharide has excellent antioxidant and anti-ultraviolet radiation effects besides the common water-locking and moisturizing effects, and can protect the skin and isolate external irritation, inflammation and ultraviolet pollution. The apocynum venetum essential oil and the apocynum venetum polysaccharide are applied to the cosmetics, and under the combined action of the apocynum venetum essential oil and other components, the cosmetics have the effects of ultraviolet radiation resistance, oxidation resistance and whitening.
Drawings
FIG. 1 shows the result of the scavenging activity of Apocynum venetum polysaccharide on superoxide anion free radicals.
FIG. 2 shows the result of hydroxyl radical scavenging activity test by Apocynum venetum polysaccharide.
FIG. 3 shows the result of lipid peroxidation resisting activity of Apocynum venetum polysaccharide.
FIG. 4 shows the result of tyrosinase activity inhibition test by apocynum venetum essential oil.
Detailed Description
The invention provides a apocynum venetum extract, which comprises the effective components of apocynum venetum essential oil and apocynum venetum polysaccharide.
In the present invention, as the raw material, commercially available products known to those skilled in the art may be used unless otherwise specified.
The invention also provides a preparation method of the apocynum venetum extract in the technical scheme, which comprises the following steps:
carrying out ultrasonic extraction on the dogbane leaves to obtain a primary extract;
distilling the primary extract to obtain apocynum venetum essential oil and an extracting solution;
and filtering and extracting the extracting solution with alcohol to obtain the apocynum venetum polysaccharide.
The invention carries out ultrasonic extraction on dogbane leaves to obtain a primary extract. In the invention, the mode of ultrasonic extraction is preferably that the dogbane leaves are crushed and then added into water for ultrasonic extraction; the mass ratio of the apocynum venetum leaves to the water is 1: 10-30, the further preferable ratio is 1: 12-28, and the further preferable ratio is 1: 15-25. In the invention, the power of ultrasonic extraction is preferably 200-300W, more preferably 210-290W, and even more preferably 220-280W; in an embodiment of the invention, the power of the ultrasound extraction is specifically 250W. In the invention, the ultrasonic extraction time is preferably 60-120 min, more preferably 70-110 min, and even more preferably 80-100 min; in the embodiment of the present invention, the time of ultrasonic extraction is specifically 90 min. In the invention, the temperature of ultrasonic extraction is preferably 50-70 ℃, more preferably 52-68 ℃, and more preferably 55-65 ℃.
After the primary extract is obtained, the method distills the primary extract to obtain the apocynum venetum essential oil and the extracting solution. Steam distillation is preferably employed in the present invention. In the invention, the distillation time is preferably 2-4 h, more preferably 2.2-3.8 h, and even more preferably 2.5-3.5 h. In the invention, the volatile oil collected after distillation is the apocynum venetum essential oil, and the residual base solution is the extracting solution.
After the extracting solution is obtained, the extracting solution is filtered and extracted by alcohol to obtain the apocynum venetum polysaccharide. In the present invention, it is preferable that the extract is filtered while it is hot to obtain a supernatant.
Alcohol is preferably carried out in advance in the invention, the supernatant is preferably concentrated by distillation under reduced pressure, and the volume after concentration is preferably 1/5 of the supernatant. The invention has no special requirements on the condition parameters of the reduced pressure distillation concentration, and can obtain the concentrated solution with the required volume. In the invention, the alcohol extraction mode is preferably to add 95% ethanol into the concentrated solution, and the concentrated solution is stood and then centrifuged to obtain sediment, namely the apocynum venetum polysaccharide; the volume ratio of the ethanol to the concentrated solution is preferably 2-5: 1, more preferably 2.5-4.5: 1, and more preferably 3-4: 1; the standing time is preferably 20-30 h, more preferably 22-28 h, and even more preferably 24 h. According to the invention, the apocynum venetum essential oil and polysaccharide components can be simultaneously obtained through one-time heating water extraction process by adopting ultrasonic-assisted steam distillation-hot water coupling extraction, so that on one hand, the yield of the essential oil and the polysaccharide can be improved, and on the other hand, the preparation method is simple, convenient, efficient and energy-saving.
After the apocynum venetum polysaccharide is obtained, the apocynum venetum polysaccharide is preferably refined in a refining mode, wherein the refining mode preferably comprises enzyme hydrolysis and impurity removal. In the invention, the enzyme hydrolysis is preferably carried out by adding papain into an apocynum venetum polysaccharide solution, wherein the mass concentration of the apocynum venetum polysaccharide solution is preferably 5-10%, more preferably 6-9%, and even more preferably 7-8%; the papain accounts for 2-4 wt.%, preferably 2.5-3.5 wt.%, and more preferably 3 wt.% of the apocynum venetum polysaccharide; the enzymatic hydrolysis is preferably carried out under heated conditions; the heating mode is preferably water bath heating, and the heating temperature is preferably 40-50 ℃, more preferably 42-48 ℃, and more preferably 45 ℃; the heating time is preferably 1 to 3 hours, more preferably 1.5 to 2.5 hours, and still more preferably 2 hours.
After the enzymatic hydrolysis, the method preferably removes impurities from the hydrolyzed solution, and the method preferably comprises the steps of adding an impurity removal reagent into the solution for extraction to obtain a water phase part; in the embodiment of the invention, the impurity removal reagent is specifically chloroform and n-butanol, and the mass ratio of the chloroform to the n-butanol is preferably 3-6: 1, more preferably 3.5-5.5: 1, and more preferably 4-5: 1; the dosage of the impurity removal reagent is preferably 1/10-1/2, more preferably 1/5-2/5, and even more preferably 1/3 of the volume of the polysaccharide solution. After the water phase part is obtained, the invention preferably carries out concentration and alcohol extraction on the water phase part to obtain the apocynum venetum polysaccharide; the concentration mode is preferably vacuum distillation concentration, and the volume after concentration is 1/5 of the water phase part volume. The invention has no special requirements on the condition parameters of the reduced pressure distillation concentration, and can obtain the concentrated solution with the required volume. After the concentrated solution is obtained, the concentrated solution is preferably subjected to alcohol extraction in the invention, the alcohol extraction mode is preferably that 95% ethanol is added into the concentrated solution, the concentrated solution is kept stand and then centrifuged, and the obtained precipitate is the apocynum venetum polysaccharide; the volume ratio of the ethanol to the concentrated solution is preferably 2-5: 1, more preferably 2.5-4.5: 1, and more preferably 3-4: 1; the standing time is preferably 20-30 h, more preferably 22-28 h, and even more preferably 24 h. The apocynum venetum polysaccharide obtained after alcohol extraction is preferably dried, and the drying mode is preferably vacuum freeze drying; the invention has no special requirements on the parameters of vacuum drying, and the dried apocynum venetum polysaccharide can be obtained. The invention adopts the modes of enzymatic hydrolysis and impurity removal for refining, can effectively remove protein in the polysaccharide, and ensures that the purity of the polysaccharide is higher.
The invention also provides an anti-ultraviolet antioxidant whitening cosmetic which comprises the following components in percentage by mass: 2-12% of apocynum venetum extract, 3-8% of stearic acid, 1.5-4% of octadecanol, 1-3% of isopropyl palmitate, 3-8% of vaseline, 2-6% of white oil, 3-8% of silicone oil, 0.5-1.5% of vitamin E, 1-3% of emulsifier, 2-5% of propylene glycol, 2-5% of nano titanium dioxide, 0.5-1.5% of triethanolamine, 0.3-1.0% of phenoxyethanol and the balance of water; the apocynum venetum extract is apocynum venetum essential oil and apocynum venetum polysaccharide which are prepared by the technical scheme.
The anti-ultraviolet antioxidant whitening cosmetic provided by the invention comprises 2-12% of apocynum venetum extract, more preferably 3-11%, more preferably 4-10%, and the content of the apocynum venetum essential oil in the anti-ultraviolet antioxidant whitening cosmetic is 0.5-3%, more preferably 1-2.5%, more preferably 1.5-2%; the content of the apocynum venetum polysaccharide is 1.5-9%, more preferably 2-8.5%, and still more preferably 2.5-8%. In the invention, the apocynum venetum polysaccharide has good ultraviolet radiation resistance and oxidation resistance besides the effects of water locking and moisture retention; the apocynum venetum essential oil can inhibit the activity of tyrosinase and the generation of melanin, and has the whitening effect.
The anti-ultraviolet antioxidant whitening cosmetic provided by the invention comprises 3-8% of stearic acid by mass percentage, more preferably 3.5-7.5% of stearic acid by mass percentage, and even more preferably 4-7% of stearic acid by mass percentage. In the invention, the stearic acid can play a role in lubrication and emulsification, and can change the cosmetics into a stable white paste.
The ultraviolet-resistant, antioxidant and whitening cosmetic provided by the invention comprises 1.5-4% of octadecanol, more preferably 2-3.5%, and even more preferably 2.5-3% by mass. In the invention, the octadecanol is a skin conditioner and an emulsion stabilizer.
The ultraviolet-resistant, antioxidant and whitening cosmetic provided by the invention comprises 1-3% of isopropyl palmitate, more preferably 1.2-2.8%, and even more preferably 1.5-2.5% by mass. In the invention, the isopropyl palmitate can increase the ductility of the cosmetic, so that the cosmetic is fine, smooth, bright and non-greasy.
The uvioresistant, antioxidant and whitening cosmetic provided by the invention comprises, by mass, 3-8% of vaseline, more preferably 3.5-7.5%, and even more preferably 4-7%. In the invention, the vaseline can play a role in moisturizing and nourishing the skin.
The anti-ultraviolet antioxidant whitening cosmetic provided by the invention comprises, by mass, 2-6% of white oil, more preferably 2.5-5.5%, and even more preferably 3-5%. In the invention, the white oil can block the moisture evaporation of the skin and plays a role in lubrication and moisture preservation in cosmetics.
The ultraviolet-resistant, antioxidant and whitening cosmetic provided by the invention comprises 3-8% of silicone oil by mass, more preferably 3.5-7.5% of silicone oil by mass, and even more preferably 4-7% of silicone oil by mass. In the invention, the silicone oil can play a moisturizing and lubricating role in cosmetics, can regulate skin feel and enables the cosmetics to be pushed away more easily.
The anti-ultraviolet antioxidant whitening cosmetic provided by the invention comprises, by mass, 0.5-1.5% of vitamin E, more preferably 0.6-1.4%, and even more preferably 0.7-1.3%. In the present invention, the vitamin E can accelerate skin metabolism, promote skin repair and regeneration.
The ultraviolet-resistant, antioxidant and whitening cosmetic provided by the invention comprises 1-3% of emulsifier by mass, more preferably 1.2-2.8% by mass, and even more preferably 1.5-2.5% by mass. In the invention, the emulsifier can emulsify the essential oil components in the cosmetic, so that the essential oil is more stable in the cosmetic.
The anti-ultraviolet, antioxidant and whitening cosmetic provided by the invention comprises 2-5% of propylene glycol, more preferably 2.5-4.5%, and even more preferably 3-4% by mass. In the present invention, the propylene glycol is capable of keeping the skin moist.
The anti-ultraviolet antioxidant whitening cosmetic provided by the invention comprises 2-5% of nano titanium dioxide by mass, more preferably 2.5-4.5% by mass, and even more preferably 3-4% by mass. In the invention, the nano titanium dioxide is used as a physical sun-screening agent to absorb and obstruct ultraviolet rays.
The ultraviolet-resistant, antioxidant and whitening cosmetic provided by the invention comprises, by mass, 0.5-1.5% of triethanolamine, more preferably 0.6-1.4%, and even more preferably 0.7-1.3%. In the invention, the triethanolamine is used as an emulsifier and a humectant, so that the cream of the cosmetic is fine and smooth and is bright and white.
The anti-ultraviolet, antioxidant and whitening cosmetic provided by the invention comprises, by mass, 0.3-1.0% of phenoxyethanol, more preferably 0.4-0.9%, and even more preferably 0.5-0.8%. In the invention, the phenoxyethanol can play a role of a preservative.
The invention also provides the application of the apocynum venetum extract in the ultraviolet radiation resistant, antioxidant and whitening cosmetics.
The invention also provides a preparation method of the ultraviolet-resistant, antioxidant and whitening cosmetic, which comprises the following steps:
mixing stearic acid, octadecanol, isopropyl palmitate, vaseline, white oil, silicone oil, vitamin E and an emulsifier to obtain an oil phase system;
dispersing propylene glycol, nano titanium dioxide, apocynum venetum polysaccharide and triethanolamine in water to obtain a water phase system;
and mixing the oil phase system and the water phase system with the apocynum venetum essential oil and the phenoxyethanol to obtain the anti-ultraviolet anti-oxidation whitening cosmetic.
The oil phase system is obtained by mixing stearic acid, octadecanol, isopropyl palmitate, vaseline, white oil, silicone oil, vitamin E and an emulsifier.
Preferably, stearic acid, octadecanol, isopropyl palmitate and vaseline are mixed and stirred uniformly under the heating condition; in the invention, the heating temperature is preferably 60-75 ℃, more preferably 62-73 ℃, and more preferably 65-70 ℃; the invention has no special requirement on the stirring condition and can be mixed uniformly. After uniformly mixing, preferably adding white oil, silicone oil, vitamin E and an emulsifier, and uniformly stirring under a heating condition; in the invention, the heating temperature is preferably 85-95 ℃, more preferably 87-93 ℃, more preferably 85-90 ℃, and the stirring time is preferably 15-30 min, more preferably 18-27 min, more preferably 20-25 min. After uniformly stirring, preferably cooling the mixture to 65-75 ℃ to obtain an oil phase system. Mixing at the above temperatures can make the components in the oil phase system more miscible with each other.
The invention disperses propylene glycol, nanometer titanium dioxide, apocynum venetum polysaccharide and triethanolamine in water to obtain a water phase system.
The invention preferably disperses propylene glycol, nano titanium dioxide and apocynum venetum polysaccharide in water, and the mixture is stirred uniformly under the heating condition; in the invention, the heating temperature is preferably 45-60 ℃, more preferably 47-58 ℃, and more preferably 45-55 ℃; after uniformly stirring, preferably heating to 65-75 ℃ under the stirring condition, and adding triethanolamine to obtain a water phase system. The emulsifying effect of the aqueous system can be improved at the above temperature.
The anti-ultraviolet antioxidant whitening cosmetic is prepared by mixing the oil phase system, the water phase system, the apocynum venetum essential oil and phenoxyethanol. Preferably, the oil phase system and the water phase system are mixed at 65-75 ℃, the mixture is uniformly stirred, after the temperature of the system is reduced to 50-60 ℃, the apocynum venetum essential oil is added and uniformly stirred, and phenoxyethanol is added to obtain the anti-ultraviolet, anti-oxidation and whitening cosmetic. In the invention, the preparation process can prevent the volatilization of the essential oil and can enable the components to be better emulsified in the product.
In order to further illustrate the present invention, the apocynum venetum extract and the ultraviolet-resistant, antioxidant and whitening cosmetic provided by the present invention will be described in detail below with reference to the accompanying drawings and examples, which should not be construed as limiting the scope of the present invention.
Example 1
Pulverizing folium Apocyni Veneti, adding deionized water at a mass ratio of 1: 20, and performing ultrasonic treatment at 60 deg.C under 250W for 90min to obtain primary extract.
And (3) carrying out steam distillation on the primary extract for 4 hours, wherein the collected volatile oil is the apocynum venetum essential oil, the residual base solution is the extracting solution, and the extraction rate of the apocynum venetum essential oil is 0.12-0.14%.
Filtering the hot extract, distilling the supernatant under reduced pressure, concentrating to 1/5 volume of the supernatant to obtain concentrated solution, adding 95% ethanol 4 times of the volume of the concentrated solution, standing for 24 hr, and centrifuging to obtain precipitate, i.e. herba Apocyni Veneti polysaccharide.
Preparing apocynum venetum polysaccharide into a solution with the mass concentration of 6%, and adding 3 wt.% of papain; heating in water bath at 45 deg.C for 2 hr, adding impurity removing agent (mass ratio of chloroform to n-butanol is 5: 1) of polysaccharide solution volume 1/3, and extracting to obtain water phase. Distilling and concentrating the water phase part to 1/5 volume, adding 95% ethanol 4 times of the concentrated solution volume, standing for 24 hr, centrifuging, and vacuum freeze drying the precipitate to obtain Apocynum venetum polysaccharide.
Example 2
Preparing the anti-ultraviolet, anti-oxidation and whitening cosmetic from the apocynum venetum polysaccharide obtained in the example 1 and the apocynum venetum essential oil according to the following formula components: 5% of stearic acid, 2.5% of octadecanol, 1.5% of isopropyl palmitate, 5% of vaseline, 4% of white oil, 5% of silicone oil, 1% of vitamin E, 2% of apocynum venetum essential oil, 2% of emulsifier, 3% of propylene glycol, 5% of apocynum venetum polysaccharide, 3% of nano titanium dioxide, 1% of triethanolamine, 0.5% of phenoxyethanol and the balance of deionized water.
Mixing stearic acid, octadecanol, isopropyl palmitate and vaseline, and stirring uniformly at 65 ℃; adding white oil, silicone oil, vitamin E and emulsifier, stirring at 90 deg.C for 25min, and cooling to 70 deg.C to obtain oil phase system; dispersing propylene glycol, nano titanium dioxide and apocynum venetum polysaccharide in water, and uniformly stirring at 50 ℃; heating to 70 deg.C, adding triethanolamine to obtain water phase system.
Mixing the oil phase system and the water phase system at 70 deg.C, cooling to 55 deg.C, adding herba Apocyni Veneti essential oil, stirring, and adding phenoxyethanol to obtain the final product.
Example 3
Preparing the anti-ultraviolet, anti-oxidation and whitening cosmetic from the apocynum venetum polysaccharide obtained in the example 1 and the apocynum venetum essential oil according to the following formula components: 3% of stearic acid, 4% of octadecanol, 1% of isopropyl palmitate, 8% of vaseline, 2% of white oil, 8% of silicone oil, 0.5% of vitamin E, 3% of apocynum venetum essential oil, 3% of emulsifier, 5% of propylene glycol, 2% of apocynum venetum polysaccharide, 5% of nano titanium dioxide, 0.5% of triethanolamine, 0.3% of phenoxyethanol and the balance of deionized water.
Mixing stearic acid, octadecanol, isopropyl palmitate and vaseline, and stirring uniformly at 60 ℃; adding white oil, silicone oil, vitamin E and emulsifier, stirring at 85 deg.C for 30min, and cooling to 65 deg.C to obtain oil phase system; dispersing propylene glycol, nano titanium dioxide and apocynum venetum polysaccharide in water, and uniformly stirring at 45 ℃; heating to 65 ℃, and adding triethanolamine to obtain a water phase system.
Mixing the oil phase system and the water phase system at 65 deg.C, cooling to 50 deg.C, adding herba Apocyni Veneti essential oil, stirring, and adding phenoxyethanol to obtain the final product.
Example 4
Preparing the anti-ultraviolet, anti-oxidation and whitening cosmetic from the apocynum venetum polysaccharide obtained in the example 1 and the apocynum venetum essential oil according to the following formula components: 8% of stearic acid, 1.5% of octadecanol, 3% of isopropyl palmitate, 3% of vaseline, 6% of white oil, 3% of silicone oil, 1.5% of vitamin E, 0.5% of apocynum venetum essential oil, 1% of emulsifier, 2% of propylene glycol, 8% of apocynum venetum polysaccharide, 2% of nano titanium dioxide, 1.5% of triethanolamine, 1.0% of phenoxyethanol and the balance of deionized water.
Mixing stearic acid, octadecanol, isopropyl palmitate and vaseline, and stirring uniformly at 75 ℃; adding white oil, silicone oil, vitamin E and emulsifier, stirring at 95 deg.C for 15min, and cooling to 75 deg.C to obtain oil phase system; dispersing propylene glycol, nano titanium dioxide and apocynum venetum polysaccharide in water, and uniformly stirring at 60 ℃; heating to 75 deg.C, adding triethanolamine to obtain water phase system.
Mixing the oil phase system and the water phase system at 75 deg.C, cooling to 60 deg.C, adding herba Apocyni Veneti essential oil, stirring, and adding phenoxyethanol to obtain the final product.
And (3) verifying the antioxidant performance of the apocynum venetum polysaccharide:
example 5
The apocynum venetum polysaccharide obtained in example 1 was subjected to an activity measurement experiment for scavenging superoxide anion radicals.
Preparing apocynum venetum polysaccharide solutions with mass concentrations of 0.2, 0.4, 0.6, 0.8 and 1.0mg/mL, precisely measuring 6.50mL of 0.05mol/L Tris-HCl buffer solution (pH 8.2), placing in a water bath at 25 ℃, preheating for 20min, respectively adding 1.00mL of apocynum venetum polysaccharide solutions with different concentrations and 0.40mL of 25mmol/L pyrogallol solution, mixing uniformly, placing in a water bath at 25 ℃ for reaction for 5min, and adding 1.00mL of 8mmol/L HCl solution to terminate the reaction. The absorbance was measured at a wavelength of 325 nm. Triplicate samples were taken for each sample and the mean value was A3. The positive control is vitamin C, and corresponding background absorbance values A1, A2 and A4 are respectively determined by referring to the operation, and the superoxide anion clearance rate is calculated according to the following formula:
clearance { [ (a1-a2) - (A3-a4) ]/(a1-a2) } 100%
A1: absorbance value without sample;
a2: absorbance values without sample and pyrogallol;
a3: (ii) an absorbance value comprising the sample and pyrogallol;
a4: absorbance values with sample, but no pyrogallol.
The results of the scavenging activity test of apocynum venetum polysaccharide on superoxide anion free radicals are shown in table 1 and fig. 1.
TABLE 1 Apocynum venetum polysaccharide scavenging activity test results for superoxide anion radical
As can be seen from Table 1, in the experimental concentration range, with the increase of the concentrations of vitamin C and apocynum venetum polysaccharide, the clearance rates of vitamin C and apocynum venetum polysaccharide to superoxide anion free radicals are also obviously increased, and the median Inhibitory Concentration (IC) of the apocynum venetum polysaccharide is also obviously increased50) A value of about 0.38mg/mL, slightly above the median inhibitory concentration of vitamin C (0.28 mg/mL); this indicates that the scavenging activity of the apocynum venetum polysaccharide and the vitamin C on superoxide anion free radicals is in the same order of magnitude.
Example 6
The apocynum venetum polysaccharide obtained in example 1 was subjected to an activity measurement experiment for scavenging hydroxyl radicals.
Preparing apocynum venetum polysaccharide solution with mass concentration of 0.2, 0.4, 0.6, 0.8 and 1.0mg/mL, and adopting improved Smimoff salicylic acid method, namely, LilyBy H2O2With Fe2+The reaction generates hydroxyl radical, salicylic acid is added into the system to capture the hydroxyl radical and generate a colored substance, and the substance has maximum absorption at 510 nm. 10mL test tubes with plugs were used, 10m mol/L FeSO was added to each tube41mL of each solution and 10mmol/L salicylic acid solution and 1mL of apocynum venetum polysaccharide solution with different concentrations, and finally adding 9mmol/L H2O2The reaction was started with 1mL of the solution, and distilled water was added to 10mL of the solution, and after the reaction was carried out in a water bath at 37 ℃ for 30min, the absorbance at 510nm was measured by zeroing with distilled water. Three replicates of each sample were taken and averaged for a 1. The positive control is vitamin C, and the corresponding background absorbance value A2 is respectively determined by referring to the operations, and the hydroxyl radical clearance rate is calculated according to the following formula:
clearance ═ 1- (a1-a2)/a0 × 100%
A0: adding the sample into the system without adding the sample, namely replacing the sample with 1mL of distilled water;
a1: sample adding reaction;
a2: adding sample but not reacting, i.e. replacing H with 1mL of distilled water2O2The solution was added to the system.
The results of the test for the scavenging activity of apocynum venetum polysaccharide on the super hydroxyl radical are shown in table 2 and fig. 2.
TABLE 2 Apocynum venetum polysaccharide hydroxyl radical scavenging Activity test results
As can be seen from Table 2, with the increase of the concentration, the effect of eliminating hydroxyl free radicals of the apocynum venetum polysaccharide is obvious, and the elimination capability and the concentration have obvious dose-effect relationship, namely IC50The value is almost equal to that of the vitamin C, which indicates that the apocynum venetum polysaccharide obtained by the invention has the capability of eliminating hydroxyl free radicals equivalent to that of the vitamin C.
Example 7
The apocynum venetum polysaccharide obtained in example 1 was subjected to an anti-lipid peroxidation activity assay.
Preparing apocynum venetum polysaccharide solutions with mass concentrations of 0.2, 0.4, 0.6, 0.8 and 1.0mg/mL, precisely measuring 0.50mL of lecithin solution, adding 1.00mL of PBS buffer solution with the pH value of 7.4, 1.00mL of apocynum venetum polysaccharide solution with different concentrations and 1.00mL of 2.5mmol/L EDTA-Fe (II), uniformly mixing, reacting in a water bath at 37 ℃ for 45min, adding 2.00mL of 28% (w/v) trichloroacetic acid and 1.00mL of 1% (w/v) thiobarbituric acid, uniformly mixing, placing in a boiling water bath at 100 ℃ for heating for 10min, cooling, and measuring the absorbance at 532 nm. The absorbance A0 was measured by zeroing with PBS buffer and replacing the sample with PBS buffer for blank tubes. Three replicates of each sample were taken and averaged for a 1. The positive control is vitamin C. The lipid peroxidation inhibition was calculated as follows:
inhibition (%) - (a0-a1)/a 0%
A0: absorbance without sample;
a1: including the absorbance of the sample.
The results of the anti-lipid peroxidation activity test of the apocynum venetum polysaccharide are shown in table 3 and fig. 3.
TABLE 3 Apocynum venetum polysaccharide anti-lipid peroxidation Activity test results
As can be seen from Table 3, Apocynum venetum polysaccharide vs. Fe2+The induced peroxidation of the lecithin liposome has an inhibiting effect, and the inhibition rate is slowly increased along with the increase of the concentration and is equivalent to the inhibition rate of vitamin C on the lipid peroxidation.
Superoxide anion free radicals are harmful free radicals closely related to the human body, attack biological macromolecules, cause the crosslinking or the breakage of the biological macromolecules, cause the destruction of cell structures and functions and cause aging; hydroxyl free radical is the most active free radical in human body with the greatest harm to organism, and can react with lipid, polypeptide, protein, DNA and the like to initiate the oxidation of unsaturated fatty acid to form Lipid Peroxide (LPO), destroy the membrane structure, cause the damage of cells and tissues and organs, induce various diseases and accelerate the aging of organism; lipid peroxidation can damage biological membranes and their functions, leading to cell transparency lesion, fibrosis, and extensive cell damage leading to damage to skin, nerves, tissues, organs, etc. As can be seen from tables 1 to 3, the apocynum venetum polysaccharide has good scavenging capacity for superoxide anion free radicals and hydroxyl free radicals, has good inhibition effect on lipid peroxidation, and has excellent in-vitro antioxidant activity.
And (3) verification of the ultraviolet radiation resistance of the apocynum venetum polysaccharide:
example 8
The apocynum venetum polysaccharide obtained in example 1 is subjected to an anti-ultraviolet radiation test, and an in vitro radiation test is performed by using escherichia coli as a model thallus to detect the anti-ultraviolet radiation protection effect of the apocynum venetum polysaccharide.
1. Preparation of suspension liquid
The frozen seed was removed and prepared in sterile test tubes (with stoppered plugs), sterilized LB broth and pipette. In a clean bench, firstly adding 1/2 LB liquid culture medium into a test tube with a plug, then adding 0.5mL of strain into the test tube by using a liquid transfer gun, finally covering the test tube with the plug, putting the test tube into a shaking table for culturing for 18h-24h at 37 ℃ and 180rpm, and taking out the test tube and refrigerating the test tube for later use.
2. Preparation of polysaccharide solutions of different concentrations
Accurately weighing 5g of apocynum venetum polysaccharide powder, dissolving the apocynum venetum polysaccharide powder in 100mL of sterile physiological saline to prepare a solution with the concentration of 5%, diluting ten times to obtain a 0.5% solution, and refrigerating the solution for later use.
3. Preparation of solid nutrient agar medium
Accurately weighing 10g of tryptone, 5g of yeast extract, 10g of sodium chloride and 20g of agar powder, putting the weighed materials into a beaker, adding 1000mL of distilled water into the beaker, heating and stirring the materials to fully dissolve the materials, pouring the materials into a conical flask for sealing, putting the conical flask into an autoclave for sterilization at 121 ℃ for 20min, subpackaging the materials after the sterilization is finished, pouring the materials into a sterilization flat plate, and putting the sterilized flat plate into a refrigerator for cold storage after complete cooling and solidification for later use.
4. In vitro thallus radiation experiment
Taking three sterilized plates, adding 1mL of the previously prepared bacterial suspension into each plate by using a pipette, adding 9mL of apocynum venetum polysaccharide solutions with different concentrations into two plates respectively, and adding 9mL of sterile physiological saline as a blank control group. And (3) after fully mixing, placing the flat plate under an ultraviolet lamp, starting timing from the turning on of the ultraviolet lamp, and stopping timing when the ultraviolet lamp is turned off. Respectively taking out 100 mu L of mixed bacteria liquid from the flat plates irradiated by ultraviolet light at different time, gradually diluting the mixed bacteria liquid by using sterile normal saline according to different concentration requirements, and finally taking 20 mu L of the diluted mixed bacteria liquid by using a pipette and respectively adding the mixed bacteria liquid into the nutrient agar culture medium flat plates marked correspondingly. And finally, putting the culture medium plate added with the mixed bacterial liquid into an incubator to be cultured for 24 hours at 37 ℃.
Through observation results, the optimal dilution multiple of the bacterial suspension is determined to be 103And the ultraviolet irradiation time is 0min, 5min, 10min and 15min, and the change of the number of the viable bacteria is observed under the condition. The experimental parameter design is shown in table 4, and the experimental results are shown in table 5.
TABLE 4 anti-ultraviolet radiation experimental design of mixed bacteria liquid of Escherichia coli
Serial number of culture dish | Dilution factor | Irradiation time/min | Adding sugar solution to obtain sugar solution | Sterile |
1 | 0 | √ | ||
2 | 5 | √ | ||
3 | 10 | √ | ||
4 | 15 | √ | ||
5 | 103 | 0 | 0.5% | |
6 | 103 | 5 | 0.5% | |
7 | 103 | 10 | 0.5% | |
8 | 103 | 15 | 0.5% | |
9 | 103 | 0 | 5% | |
10 | 103 | 5 | 5% | |
11 | 103 | 10 | 5% | |
12 | 103 | 15 | 5% |
TABLE 5 ultraviolet radiation resistance test results of Escherichia coli mixed bacteria liquid
Note: the number of colonies represented by ≥ 20, + represents ≥ 10, + represents ≥ 5, -represents the number of colonies visible without the naked eye.
As is apparent from Table 5, only a few surviving E.coli cells remained in the blank control group after 5min of UV irradiation, and no surviving E.coli cells remained on the medium after 10 min. In the apocynum venetum polysaccharide solution group with the concentration of 0.5%, the survival number of escherichia coli is also reduced step by step obviously from the culture medium in three time periods of 5min, 10min and 15min, but the escherichia coli still survives on the culture medium after the irradiation for 15 min. In the case of the apocynum venetum polysaccharide solution group having a concentration of 5%, the number of E.coli cells was gradually decreased in the culture medium in three periods of 5min, 10min and 15min, but a large number of viable E.coli cells remained in the culture medium even after 15min of irradiation. In conclusion, the apocynum venetum polysaccharide solution is irradiated by ultraviolet rays under the same environment and time, the protection effect on the ultraviolet radiation resistance of escherichia coli is presented, and the effect is increased along with the increase of the concentration.
And (3) verifying the performance of the apocynum venetum essential oil for inhibiting tyrosinase:
example 9
The apocynum venetum essential oil obtained in example 1 was subjected to tyrosinase inhibition test.
1. Reagent preparation
Sodium phosphate buffer (1/15M, pH 6.8): 1.0001g of sodium dihydrogen phosphate and 1.1860g of disodium hydrogen phosphate are accurately weighed, a small amount of deionized water is added for dissolution, the volume is determined to be 500mL, and the mixture is stored in a refrigerator at 4 ℃ for later use.
L-tyrosine solution (7.5 mmol/L): 0.2721g of L-tyrosine is accurately weighed, a plurality of drops of concentrated hydrochloric acid are firstly added, about 50mL of deionized water is added, after the concentrated hydrochloric acid and the deionized water are completely dissolved by slight heating, the pH value is adjusted to 7.0 by using sodium hydroxide solution, and the deionized water is added to a constant volume of 200 mL.
Test solution: accurately weighing 0.1000g of apocynum venetum essential oil, dissolving in 20mL of dimethyl sulfoxide to obtain a solution to be detected of 5mg/mL, and diluting to 2.5mg/mL, 1.25mg/mL, 0.625mg/mL, 0.3125mg/mL and 0.15625mg/mL in a double way.
Positive control (+ CK): accurately weighing 0.1000g arbutin powder, dissolving in 20mL deionized water to obtain 5.00mg/mL positive control mother liquor, and diluting to 2.5mg/mL, 1.2500mg/mL, 0.6250mg/mL, 0.3125mg/mL, 0.1562 mg/mL.
2. Preparation of tyrosinase liquid
Cleaning potato, and precooling at 4 deg.C for about 4 h. Peeled, cut into pieces of about 1X 1cm3, and frozen at-20 ℃ overnight. Adding 4 deg.C pre-cooled sodium phosphate buffer solution at a ratio of 1: 1 (W: V), homogenizing with tissue triturator, filtering with 3 layers of gauze, centrifuging the filtrate at 4000r/min for 10min to obtain supernatant as obtained tyrosinase crude enzyme solution, storing at 4 deg.C, and using up in 2 hr.
3. Inhibition of tyrosinase activity by samples
Adding phosphate buffer solution, test solution with different concentration gradients (including positive control), and enzyme solution into the test tube, and water-bathing at 30 deg.C for 10 min. The substrate L-tyrosine was then added and the timer was started immediately. The absorbance at a wavelength of 475nm at 20min of the reaction was determined. When in measurement, the inhibition rate of the test solution (including a positive control) on tyrosinase is calculated by using a corresponding negative control as a reference through the following formula, and the half Inhibition Concentration (IC) is estimated according to a concentration-enzyme inhibition rate curve50) An approximation of (d). Each experiment was performed in 3 replicates. The experimental parameter settings of the inhibition of tyrosinase activity by apocynum venetum essential oil are shown in Table 6, and the test results are shown in Table 7 andas shown in fig. 4.
Inhibition rate [ (A-B)/A ] 100%
Wherein "A" is the absorbance of the standard control and "B" is the absorbance of the test solution (or positive control).
TABLE 6 test parameter design for inhibition of tyrosinase activity by apocynum venetum essential oil
TABLE 7 Apocynum venetum essential oil tyrosinase inhibitory activity test results
As can be seen from Table 7, the inhibition rate of tyrosinase by the samples and the positive control showed an increasing trend with increasing concentration in the experimental concentration range, and the inhibition rate showed dose-dependent inhibition. In the experimental concentration range, the inhibition rate of apocynum venetum essential oil on tyrosinase is obviously higher than that of arbutin.
Example 10
The ultraviolet-resistant, antioxidant and whitening cosmetic obtained in example 2 is used for volunteer trial tests.
The test population: 20 volunteers, all female, were 18-55 years old, healthy, for 30 days.
The sunscreen cosmetic is applied to the exposed skin 15min before going out, and is applied again after 3 h. The results of the trial are shown in Table 8.
TABLE 8 trial results of ultraviolet-resistant, antioxidant, and whitening cosmetics
As can be seen from Table 8, after 30 days of trial, all the tested persons did not find red itch and irritation reaction, and the self-describing feeling was smooth and comfortable, without greasy feeling, and especially suitable for use in summer.
As can be seen from the above examples, the apocynum venetum polysaccharide has excellent in vitro oxidation resistance and ultraviolet radiation resistance, and the apocynum venetum essential oil can inhibit the activity of tyrosinase. The cosmetic added with the apocynum venetum polysaccharide and the apocynum venetum essential oil can control the generation of melanin, has the whitening effect, can actively protect the skin of a human body, isolate the skin aging problem and the like caused by external stimulation, inflammation, ultraviolet pollution and the like, and can keep the skin in a relatively durable moist and healthy state.
Although the above embodiments have been described in detail, they are only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and all of the embodiments belong to the protection scope of the present invention.
Claims (10)
1. An herba Apocyni Veneti extract contains herba Apocyni Veneti essential oil and herba Apocyni Veneti polysaccharide as effective components.
2. A method for preparing an apocynum venetum extract as claimed in claim 1, comprising the steps of:
carrying out ultrasonic extraction on the dogbane leaves to obtain a primary extract;
distilling the primary extract to obtain apocynum venetum essential oil and an extracting solution;
and filtering and extracting the extracting solution with alcohol to obtain the apocynum venetum polysaccharide.
3. The preparation method according to claim 2, wherein the power of ultrasonic extraction is 200-300W, the time is 60-120 min, and the temperature is 50-70 ℃.
4. The preparation method according to claim 2, wherein the distillation is steam distillation, and the distillation time is 2-4 h.
5. The method according to claim 2, wherein the preparation of the apocynum venetum polysaccharide further comprises refining the apocynum venetum polysaccharide, wherein the refining comprises enzymatic hydrolysis and impurity removal.
6. The preparation method according to claim 5, wherein the impurity removing reagent is chloroform and n-butanol, and the mass ratio of the chloroform to the n-butanol is 3-6: 1.
7. Use of the apocynum venetum extract as defined in claim 1 or obtained by the preparation method as defined in any one of claims 2 to 6 in anti-ultraviolet radiation, anti-oxidation and whitening cosmetics.
8. An anti-ultraviolet antioxidant whitening cosmetic comprises the following components in percentage by mass: 2-12% of apocynum venetum extract, 3-8% of stearic acid, 1.5-4% of octadecanol, 1-3% of isopropyl palmitate, 3-8% of vaseline, 2-6% of white oil, 3-8% of silicone oil, 0.5-1.5% of vitamin E, 1-3% of emulsifier, 2-5% of propylene glycol, 2-5% of nano titanium dioxide, 0.5-1.5% of triethanolamine, 0.3-1.0% of phenoxyethanol and the balance of water;
the apocynum venetum extract is the apocynum venetum extract disclosed by claim 1 or obtained by the preparation method disclosed by any one of claims 2 to 6.
9. The ultraviolet-resistant, antioxidant and whitening cosmetic as claimed in claim 8, wherein the content of apocynum venetum essential oil in the ultraviolet-resistant, antioxidant and whitening cosmetic is 0.5-3%, and the content of apocynum venetum polysaccharide in the cosmetic is 1.5-9%.
10. The method for preparing the ultraviolet resistant, sun-screening and whitening cosmetic as claimed in claim 8, comprising the steps of:
mixing stearic acid, octadecanol, isopropyl palmitate, vaseline, white oil, silicone oil, vitamin E and an emulsifier to obtain an oil phase system;
dispersing propylene glycol, nano titanium dioxide, apocynum venetum polysaccharide and triethanolamine in water to obtain a water phase system;
and mixing the oil phase system and the water phase system with the apocynum venetum essential oil and the phenoxyethanol to obtain the anti-ultraviolet anti-oxidation whitening cosmetic.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110045678.1A CN112516014B (en) | 2021-01-08 | 2021-01-08 | Apocynum venetum extract, preparation method thereof, anti-ultraviolet, anti-oxidation and whitening cosmetic and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110045678.1A CN112516014B (en) | 2021-01-08 | 2021-01-08 | Apocynum venetum extract, preparation method thereof, anti-ultraviolet, anti-oxidation and whitening cosmetic and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN112516014A true CN112516014A (en) | 2021-03-19 |
CN112516014B CN112516014B (en) | 2023-04-14 |
Family
ID=74977494
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110045678.1A Active CN112516014B (en) | 2021-01-08 | 2021-01-08 | Apocynum venetum extract, preparation method thereof, anti-ultraviolet, anti-oxidation and whitening cosmetic and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112516014B (en) |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006160668A (en) * | 2004-12-08 | 2006-06-22 | Sanei Gen Ffi Inc | Lipid peroxide production inhibitor |
CN101966139A (en) * | 2010-10-26 | 2011-02-09 | 戈宝绿业(深圳)有限公司 | Apocynum venetum extract, preparation method thereof and application thereof to cosmetics |
CN103169632A (en) * | 2011-12-22 | 2013-06-26 | 黄玉良 | Application of dogbane leaf extract in preparation of skin-care product |
CN110960457A (en) * | 2019-12-11 | 2020-04-07 | 香港科技大学深圳研究院 | Preparation method of apocynum venetum extract and application of apocynum venetum extract in whitening and skin-care products |
-
2021
- 2021-01-08 CN CN202110045678.1A patent/CN112516014B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006160668A (en) * | 2004-12-08 | 2006-06-22 | Sanei Gen Ffi Inc | Lipid peroxide production inhibitor |
CN101966139A (en) * | 2010-10-26 | 2011-02-09 | 戈宝绿业(深圳)有限公司 | Apocynum venetum extract, preparation method thereof and application thereof to cosmetics |
CN103169632A (en) * | 2011-12-22 | 2013-06-26 | 黄玉良 | Application of dogbane leaf extract in preparation of skin-care product |
CN110960457A (en) * | 2019-12-11 | 2020-04-07 | 香港科技大学深圳研究院 | Preparation method of apocynum venetum extract and application of apocynum venetum extract in whitening and skin-care products |
Non-Patent Citations (3)
Title |
---|
周春玲等: ""GC-MS 分析罗布麻叶挥发油的化学成分"", 《中成药》 * |
田立等: ""罗布麻多糖成分体外抗氧化活性研究"", 《中兽医医药杂质》 * |
陈斌: ""植物多糖在化妆品中的应用研究进展"", 《中国野生植物资源》 * |
Also Published As
Publication number | Publication date |
---|---|
CN112516014B (en) | 2023-04-14 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
KR100964723B1 (en) | Cosmetic composition containing wild flower extracts | |
KR20110108686A (en) | Antioxidant containing extracts of natural materials and composition of feed, food or cosmetic | |
KR100863890B1 (en) | Cosmetic composition containing extracts of inonotus obliquus, fomitopsis officinalis, agarikus blazei murill and hericium erinaceum | |
JP4567278B2 (en) | Skin cosmetics | |
KR20090096256A (en) | A method for producing extract of fermented fucoxanthin and Cosmetic composition containing thereof | |
KR100793019B1 (en) | Cosmetic composition containing an extract of Lespedeza bicolor Turcz., Glechoma hederacea var. longituba Nakai and Portulaca grandiflora Hooker for anti-oxidative and anti-inflammatory activity | |
KR100953278B1 (en) | Cosmetic composition | |
KR20040110441A (en) | Cosmetic composition containing mixture extract of OUGIDAN(Paecilomyces japonica, Acanthopanax senticosus, Ganoderam Lucidum, Deer antlers and Ginseng), and the method of manufacturing thereof with supercritical fluids extraction | |
KR20090104156A (en) | Cosmetic composition with the calming effect for skins | |
KR102101949B1 (en) | A skin-care agent or cosmetics containig Antrodia camphorata fruit body extract or Antrodia camphorata mycelium extract | |
KR101370990B1 (en) | Anti-heat aging effect of fermented Limonia acidissima extract and its cosmetic usage to improve skin problems | |
JP4906179B2 (en) | Topical skin preparation | |
CN112516014B (en) | Apocynum venetum extract, preparation method thereof, anti-ultraviolet, anti-oxidation and whitening cosmetic and preparation method thereof | |
CN110613643A (en) | Repair wrinkle-removing cream and preparation method thereof | |
KR102067283B1 (en) | A skin-care agent or cosmetics containig Morchella esculenta fruit body extract or Morchella esculenta mycelium extract | |
JP2003012532A (en) | Hyaluronidase inhibitor, hexosaminidase liberation inhibitor, cyclic amp phosphodiesterase inhibitor and cosmetic for ameliorating skin roughening | |
CN112587462B (en) | Application of coriander extract, anti-ultraviolet antioxidant whitening cosmetic and preparation method of anti-ultraviolet antioxidant whitening cosmetic | |
KR102171924B1 (en) | External skin preparation for relaxing allergy comprising extract of wild-peach and method of producing the same | |
CN114469907A (en) | Application of nerol in preparation of product for resisting skin photodamage | |
KR100532633B1 (en) | Cosmetic composition having anti-inflammatory, skin-protecting, skin-elastic effects which comprise mixed plants extract | |
CN107303255B (en) | Sorghum fermentation product having anti-inflammatory, anti-allergic and atopic skin improving effects, its preparation method and cosmetic composition | |
KR102333132B1 (en) | Cosmetic Composition containing Frangipani Oil or Fermented Frangipani Oil | |
KR102073943B1 (en) | A skin-care agent or cosmetics containig Lyophyllum ulmarium fruit body extract or Lyophyllum ulmarium mycelium extract | |
KR100580858B1 (en) | A cosmetic composition containing mixing extract of Shipjangsaeng-related natural substancePinus sylvestris, Ganoderma lucidum Karst., blueberry, Cervus elaphus L., Amyda sinensis, Germanum, Apis mellifera L., Panax ginseng C.A.Meyer, salmon egg and Citrus Medica Limonum and the method of manufacturing thereof | |
KR20150136290A (en) | Extract Of bee venom, extract of willow bark and extract of fermented rice Containing Cosmetic Composition Having Anti-aging Effect |
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 |