CN109984983A - A kind of preparation method of the composition with natural sun-prevention performance - Google Patents
A kind of preparation method of the composition with natural sun-prevention performance Download PDFInfo
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- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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Abstract
The present invention provides a kind of preparation method of composition with natural sun-prevention performance, comprising: A phase raw material is carried out sterilization processing, adjusts 75-85 DEG C of temperature, stirring is transparent to material dissolution, and A phase raw material includes water and carbomer；B phase raw material is heated to 80-90 DEG C, is stirred evenly, B phase raw material includes one or both of one or both of tristerin and PEG-100 stearate and cetostearyl alcohol olive oleate and the smooth olive oleate of sorb；B phase raw material and A phase raw material are mixed, 75-85 DEG C of temperature；Emulsifying；C phase raw material is added and is stirred evenly；C phase raw material includes triethanolamine, dendrobium candidum extract, ginger extract, Magnolia cortex P.E, angelica extract.Preparation method of the invention is simple to operation, wherein using supercritical CO2Natural plants are extracted, extraction efficiency is good, economical and energy saving environmental protection.Composition obtained is highly-safe, sun-proof ability with higher.
Description
Technical field
The present invention relates to a kind of sunscreen products, and in particular, to a kind of preparation of the composition with natural sun-prevention performance
Method.
Background technique
In recent decades, ozone layer, which constantly wrecks, causes amount of ultraviolet irradiation to gradually increase.It is well known that ultraviolet light
It is divided into 3 classes, the medium wavelength ultraviolet light (UVA) and 320- of short wave ultraviolet (UVC), 280-320nm comprising 200-200nm
The long wavelength ultraviolet light (UVB) of 400nm.UVC can be fully absorbed by atmosphere, and UVA and UVB penetrates atmosphere to the mankind's
Health, which constitutes harm, especially UVB, can lead to cutaneous pigmentation, cutin growth, light aging, or even cause cutaneum carcinoma and machine
The immunosupress of body, the irradiation of excessive UVA ultraviolet light can promote the formation of wrinkle even to cause phototoxic reaction.It is how effectively anti-
It shines to reduce the attention that the generation of skin disease has caused more and more people.In numerous sun-proof approach, can be had using sun-screening agent
Effect reduces ultraviolet light and damages to skin bring.According to sun-proof mechanism, sun-screening agent is broadly divided into chemical sun and physical sunscreen
Agent.Chemical sun mainly passes through anti-oxidant or anti-radical action, reduces the ultraviolet energy for being irradiated to skin, mitigates ultraviolet
Line radiation injury caused by skin or hair, to directly or indirectly enhance the sun-proof performance of product.Traditional chemical sun-screening agent
Sun-proof result is good, but easily causes skin irritatin, generates the side effects such as allergy, inflammation, therefore develop natural plant sun agent, no
Only safety is relatively high, can also play anti-aging, whitening, anti-inflammatory and other effects sometimes, have broad application prospects.
Studies show that, natural sun-screening agents have absorption to specific wavelength ultraviolet light, and it is smaller to skin irritation, and it has
There is good skin sense.But action component is complicated, and safety and sun-proof result all need further to be studied, but natural extract component is used
It is the trend of sun-screening agent development as sun-screening agent, requirement of the consumer to sun-screening agent also more tends to natural sun-prevention component.Mesh
It is preceding have been found that many natural plants, such as: chitin, seaweed, aloe, sea-buckthorn, ginkgo, radix scutellariae, sandlwood, vitamin E, vitamin
A, the sophora bud, the coptis, safflower, sunset abelmoschus flower, Asian puccoon, the sophora bud, cassia bark, Niu Fang, walnut, cordate houttuynia, grape, jujube, narcissus lotus, winter
Melon, Yuan rose, Chinese prickly ash, potato, herba stellariae mediae, sesame, parsley, lotus perfume (or spice) Primula malacoides, Dicentra spectabilis, camomile, chamomile, perennial root are heralded spring
The plants such as flower, cimicifugae foetidae, sky japanese bearbind, Huang slight, Siberian cocklebur, motherwort, dandelion and oriental wormwood punt-pole all have preferable ultraviolet radiation absorption and make
With.And what is played a role is natural active matter that it contains, such as: flavone compound, anthraquinone analog compound and its derivative,
Terpenoid.
Traditionally, organic solvent method or steam distillation (such as Chinese Pharmacopoeia are extracted as to active ingredient of natural plant
It is contained).Organic solvent easily brings dissolvent residual and solvent side effect, and solvent recovery is troublesome and is unfavorable for energy-saving and environmental protection.Vapor
Although the way of distillation primary property investment in production equipment is less, yield is lower and due to being extracted at 100 DEG C or more, temperature
Degree is higher, for heat-sensitive substance, is easy to happen time biochemical reaction, the component of extraction tends not to represent former plant extracts
The problems such as really composition, there is extraction time is long, yield is low；Furthermore because of high temperature boiling, in the remaining dregs of a decoction it is related chemistry at
Divide and time biochemical reaction also has occurred, cannot completely represent the real chemical composition of remainder, physical behavior also has occurred very big
Variation, recycles it also restrained.
Use supercritical CO2Natural plants are extracted, there is preferable extracting and developing efficiency, and have collection extracting and developing, concentration
Be integrated, integrated operation is at low cost, no solvent residue, it is pollution-free, energy saving, easy to operate the advantages that, applied both at home and abroad
In fields such as biochemical industry, food, medicine, environmental protection.At home, supercritical CO2Abstraction technique is in modernization of Chinese medicine process
Research and application receive more and more attention and pay attention to, and become China in the spy of supercritical fluid technique research and application field
Color, there is a prospect very much, and supercritical extraction technique has been classified as before the practical tool of modern Chinese herbal medicine well develops by China in the modernization of Chinese medicine
The new technology of scape.For the process for accelerating the modernization of Chinese medicine, supercritical CO2Abstraction technique is by State Development Planning Commission and science and technology
Portion is included in " the hi-tech industrialization major fields guide of current preference development " (1999) " Chinese materia medica preparation extraction process and dress
It is standby " in.
Extraction to natural plants, traditional method mostly uses organic solvent extraction, ultrasonic extraction etc., from extraction
The finger-print of plant extracts can be seen that supercritical CO2No matter extraction natural plants in composition diversity or extract
Effective component concentration on occupy sizable advantage, therefore this extractive technique is utilized, to the plant with sun-proof ability
It is extracted, the absorption peak showed for different plant extracts is different, by dense to its extract and its difference
The composition of the pure natural plant extract with certain sun-proof ability can be fully achieved in the compounding of degree, can effective change
Chemical synthesis sun-screening agent causes a degree of damage to human skin, be more advantageous to play Chinese tradition traditional Chinese medicine sun-proof and
The effect of cosmetic field.
A good sunscreen product will not only consider how to prevent harmful light from touching skin, it is considered however that, if
After touching skin, how to be repaired.Multi-level protection effect is formed in this way, can just be effectively protected skin from nocuousness
The damage of light.Currently, having many sunscreen products joined some natural components with after-sun restorative function come after solarization of releiving
Injury of the harmful light to human body, and this function is that traditional sun-screening agent is unexistent, this is also natural sun-screening agents to chemical sunscreen
The supplement of agent function and sound, and it is sun-proof theoretical perfect to tradition.It is contemplated that natural sun-screening agents are to chemical sun
Part replaces to whole substitutions, will be the trend and trend of sunscreen product development.
The shortcomings that prior art: firstly, according to sun-proof mechanism, sun-screening agent is broadly divided into chemical sun and physical sunscreen
Agent.Chemical sun can absorb ultraviolet light and convert thereof into energy and the release of other forms, be irradiated to skin to reduce
The ultraviolet energy of skin.Chemical sun sun-proof result is good, but easily causes skin irritatin, generates the side effects such as allergy, inflammation.
Physical sunscreen agent then passes through reflection or scatters ultraviolet plays the protective effect to skin, safety and stability, but easily blocks pore,
Influence sweat gland secretion.
Secondly, pointing out that ultraviolet filtering organic compound used in suncream carrys out coral reef according to American Studies report
Say it is a kind of noxious material, the oxybenzone (Oxybenzone) in suncream can not only kill coral living, but also to this nothing
The influence of vertebrate bring is far above this, it can also destroy the DNA of adult coral, change the DNA of childhood coral, it means that
The probability of childhood coral normal development will become very low, therefore will be particularly important using natural component sun-screening agent.
Third, skin is releived repair function after the Orangic sunscreen of conventional synthesis can not play solarization, and natural plants are extracted
And obtaining sun-prevention component not only has sun-proof ability, and SPF is higher, while there are also synergistic functions for other components.
Research finds that the antioxidant effect (or sun-proof result) of single active ingredient is often weaker than mixture, certain antioxygens
Agent is higher than activity when being used alone by its compound antioxidant activity, illustrates that there is synergistic effects between component, and help
In improving its oxidation resistance, also indicate that when playing antioxidation, between component a series of complex may occur for these substances
Reaction to improving oxidation resistance.Anti-oxidant synergistic effect refer to by carried out between different polyphenoils preferably and
Formula processing, can obtain the more oxidation resistances higher than single antioxidant, improve the oxidation stability of organism.Collaboration is made
With the synergistic effect for including intermolecular collaboration and intramolecular, Scott etc. proposes the uniform synergistic effect of intermolecular collaboration
With the concept of non-homogeneous synergistic effect.Uniform synergistic effect is that have between same mechanism but active two different compounds
Synergistic effect；Non-homogeneous synergistic effect is the synergistic effect between two or several different mechanism antioxidant.It is generally believed that antioxygen
Agent is the enzyme inactivation and shadow by removing the metal ion of free radical, complex catalysis oxidation, making catalytic oxidation in vivo
The approach such as gene expression are rung to play a role.In recent years, in antioxidant research, " the compound chain of antioxidant " it is theoretical always by
The concern of people when this theory thinks a variety of antioxidant synergy, can significantly improve activity each other, facilitate body
Keep good anti-oxidant equilibrium state.Synergistic effect between a variety of antioxidants may be constituted derived from these antioxidants
Exist between the different role position of redox cycle system or the different role mechanism of these antioxidants apparent complementary
Effect can eliminate free radical and singlet oxygen by interaction；Active oxygen and its specific action position are isolated；Change
Become oxidizing ferment or enzymatic oxidation enzymatic activity；There is provided and maintain the level of reducing agent；The reparation or substitution of molecular injury are participated in, thus
Play synergistic effect.
The bioactivity basis of substance is its chemical composition and chemical component, the bioactive functions of chemical component mainly and
Its functional group having is related, and plant extract substance has relationship between oxidation resistance genetic material and total antioxidant capacity
Research gradually increases, and has much to phenolic group substance in natural materials and flavonoids genetic material and total antioxidant capacity
Research.Phenol, flavonoid substance, organic acid, polysaccharide are all most common a few class compounds in Chinese medicine or natural plants.Phenolic substances,
As with one of strongest active constituent of oxidation resistance, there is significant prevention to make to too drastic caused many diseases are aoxidized
With, therefore generally have significant correlativity between the number and oxidation resistance of aldehydes matter content, illustrate that total phenol is anti-
Oxidability main active.In recent years, mostly several frequently seen for the research of relationship between general flavone and oxidation resistance
Flavones list material composition and certain oxidation resistance between structure-activity relationship.With the increase of general flavone content, total antioxidation
Ability has the tendency that rising, but correlation is not significant, i.e., the correlation between general flavone content and total antioxidant capacity is not
It is obvious as the related sex expression between total phenol and oxidation resistance, illustrate that certain part flavones are contributed in terms of oxidation resistance
It is not unique, organic acid, the mutual synergistic effect of polysaccharide and other microelements is common to complete the comprehensive antioxygen of an extract
Change ability.
4th, organic synthesis sun-screening agent is on preparing sunscreen product, and there are in some drawbacks and use feeling on compatibility
Glutinous soapy feeling, such as water-in-oil type sunscreen product one side thermodynamic instability, while water-in-oil type sunscreen product is brought to skin
Clouding sense, especially summer, and the sunscreen product of natural sun-screening agents preparation, either water-in-oil type or oil-in-water type produce
Product, stability and skin sense are preferable.
5th, conventional organic solvents bring dissolvent residual and solvent side effect, and solvent recovery is troublesome and is unfavorable for energy conservation, ring
It protects.Although steam distillation primary property investment in production equipment is less, yield is lower and due to being at 100 DEG C with enterprising
Row extracts, and temperature is higher, for heat-sensitive substance, is easy to happen time biochemical reaction, the component of extraction tends not to represent former plant
The problems such as real composition of object extract, there is extraction time is long, yield is low；Furthermore because of high temperature boiling, in the remaining dregs of a decoction
Time biochemical reaction also has occurred in related chemical component, cannot completely represent the real chemical composition of remainder, physical behavior
Great changes have occurred, it are recycled also restrained.This is limitation brought by conventional extraction process.
Summary of the invention
The present invention is in view of the deficienciess of the prior art, provide a kind of preparation side of composition with natural sun-prevention performance
Method can be very good to replace Synthetic Organic Chemistry sun-screening agent bring insecurity, improve on extracting process, improves extraction
Rate is taken, more perfect bioactivity is saved, while avoiding injuring to skin bring for the chemical suns such as organic synthesis, is avoided
The destruction of coralline algae or even entire ocean, biology can be very good to take by the natural plant grease of SCF-CO 2
For Synthetic Organic Chemistry sun-screening agent bring insecurity, it is good to play sun-proof result, safety, mildly, the multi-efficiency of skin care.
The technical scheme to solve the above technical problems is that
A kind of preparation method of the composition with natural sun-prevention performance, comprising the following steps:
(1) A phase raw material is subjected to sterilization processing, the rear temperature that adjusts stirs saturating to material dissolution to 75-85 DEG C
It is bright, it keeps the temperature spare；A phase raw material includes 69.95-84.24 parts and Carbopol 0.1-0.2 parts of water according to mass parts；
(2) B phase raw material is heated to 80-90 DEG C, be uniformly mixed, B phase raw material includes tristerin and PEG-
Gross mass part of one or both of 100 stearates, tristerin and PEG-100 stearate is 1-1.5 parts；B
Phase raw material further includes one or both of cetostearyl alcohol olive oleate and the smooth olive oleate of sorb, cetostearyl alcohol olive
Gross mass part of olive oleate and the smooth olive oleate of sorb is 1-1.5 parts；
(3) uniformly mixed B phase raw material is poured slowly into A phase raw material, is stirred while adding, 75-85 DEG C of temperature；
(4) above-mentioned uniformly mixed raw material is subjected to emulsifying, 75-85 DEG C of temperature；
(5) above-mentioned material is cooled down while stirring, when temperature is down to 40-50 DEG C, the object after emulsification is added in C phase raw material
It is stirred evenly in material；C phase raw material includes 0.1-0.2 parts of triethanolamine, 0.5-1 parts of dendrobium candidum extract, ginger according to mass parts
1-2 parts of extract, 1-2 parts of Magnolia cortex P.E, 2-3 parts of angelica extract.
The present invention is further arranged to, and in (1), A phase raw material further includes 3-6 mass parts glycerol and 0.05-0.1 mass
Part, part water, glycerol, allantoin and Carbopol are first heated to 80-90 DEG C in advance, heat preservation 25-40min is sterilized, after
It is cooled to the remaining glycerol of 75-85 DEG C of addition, allantoin and Carbopol, stirs, heat preservation transparent to material dissolution
It is spare.
The present invention is further arranged to, and in (2), B phase raw material further includes caprylic/capric triglyceride, the octanoic acid/last of the ten Heavenly stems
The mass parts of acid glycerol three ester are 2-4 parts.
The present invention is further arranged to, and in (2), B phase raw material further includes cetostearyl alcohol 0.2-0.5 according to mass parts
Part, 0.5-1 parts of cera alba.
The present invention is further arranged to, in (2), B phase raw material according to mass parts further include 2-4 parts of Butyrospermum parkii fruit rouge,
1-2 parts of PEG-8 dimethyl silicone polymer.
The present invention is further arranged to, and in (3), mixing speed 180-220 turns/min；In (5), mixing speed 150-
200 turns/min.
The present invention is further arranged to, and in (4), homogeneous speed 3000-5000 turns/min, homogenizing time 2-3min.
The present invention is further arranged to, and in (5), C phase raw material further includes 0.2-0.4 parts of silica according to mass parts.
The present invention is further arranged to, after C phase raw material is added, when being cooled to 30-40 DEG C, essence 0.01-0.05 parts of addition,
0.1-0.6 parts of preservative, mixing speed 150-200 turns/min, mixing time 20-30min, and rear to stop stirring, that is, preparing terminates.
The present invention is further arranged to, the extraction conditions of dendrobium candidum extract are as follows: pressure 10-20MPa, temperature 40-60
DEG C, CO2Flow 30-50L/h；The extraction conditions of ginger extract are as follows: pressure 20-30MPa, 40-60 DEG C of temperature, CO2Flow 30-
50L/h；The extraction conditions of Magnolia cortex P.E are as follows: pressure 20-30MPa, 30-50 DEG C of temperature, CO2Flow 30-50L/h；Radix Angelicae Sinensis mentions
Take the extraction conditions of object are as follows: pressure 20-30MPa, 40-60 DEG C of temperature, CO2Flow 30-50L/h.
In the composition of natural sun-prevention performance prepared by the present invention, the effect of various components is not originally: water makees solvent, sweet
Oil does moisturizer, and allantoin plays anti-irritant, and Carbopol makees thickener, and caprylic/capric triglyceride does grease moisturizing
Agent, cetostearyl alcohol play the role of assistant for emulsifying agent and thickener, and cera alba has thickening and skin sense regulator, butter
Fruit tree fruit rouge plays skin sense regulator and moisturizer, and PEG-8 dimethyl silicone polymer plays skin sense regulator and moisturizer
Effect, tristerin and PEG-100 stearate play emulsifier, and cetostearyl alcohol olive oleate and sorb are smooth
Olive oleate plays emulsifier, and triethanolamine plays pH adjusting agent, dendrobium candidum extract, ginger extract, thickness
Plain extract and angelica extract do natural sun-screening agents, and individual extract has sun-proof result, but inhales just for one
Receive under optical band, by add different plant extracts be have to guarantee natural sun-screening agents between different absorptions light it is a
It is complementary.Silica does physical sunscreen agent, and essence does odorant.
For the several plant extract selected in the present invention, it is therefore intended that from polyphenol, flavones, the main components such as polysaccharide enter
Hand cooperates, and mutually cooperates with, plays anti-oxidation efficacy jointly.Every kind of individual substance is made a concrete analysis of below.
Dendrobium officinale polysaccharide is the main component in dendrobium candidum.Polysaccharide has anti-aging, liver protection, hypoglycemic, clearing lung-heat, resists
The effects of tired.By drosophila feeding dendrobium candidum extract test, Dendrobium officinale polysaccharide extend drosophila Mean longest life,
Maximum life span, median lethal time, and the intracorporal SOD (superoxide dismutase) of drosophila is improved, it is intracorporal certainly to remove drosophila
By base and then extends the service life and enhance inverse gravity and creep ability.In addition to this, anthocyanin is that dendrobium candidum one kind has biology living
Property flavonoid substances, there is inoxidizability, remove the bioactivity such as free radical, be able to suppress inflammation, tumour, cardiovascular disease
Disease.Anthocyanin is most safe, most effective, most direct free radical in terms of prophylactic treatment disease, protection at present
One of scavenger, the ability for removing free radical is 20 times of Vc.Existing research confirms that dendrobium candidum natural pigment is anthocyanin,
And it is antibacterial with better effects to its.
The main active component of ginger is ginger oil and oleoresin ginger, and main chemical compositions are zingiberene, zingiberone and gingerol class, ginger
Phenolic compound includes 6-gingerol, 8-gingerol, 10-gingerol etc., wherein being bioactivity in ginger again with 6-gingerol content highest
The representative ingredient of substance.Research shows that 6-gingerol has a variety of medical values such as anti-oxidant, antitumor, bactericidal antiphlogistic.Including
The research of natural products and its extract antioxygenic property including ginger is the hot spot of correlative study.It is relevant the study found that
With the variation of concentration, there are some differences in low 6-gingerol content and high-purity 6-gingerol for oxidation resistance, but difference is unknown
Aobvious, theory thinks, with the increase of 6-gingerol content, oxidation resistance enhances, but in the extract of low 6-gingerol content,
Its oxidation resistance is not also poor, and illustrating different material directly has mutual synergistic function, is not one-component tool
There is good oxidation resistance.It is especially (a kind of anti-oxidant in ABTS in the oxidation resistance that concentration is 52%6- gingerol extract
Ability detection method) it is to increase with concentration and reduce in method, it is to increase in a kind of FRAP (oxidation resistance detection method) method；
9 8% high-purity 6-gingerols increase with concentration in 2 kinds of methods and are reduced, and difference is more significant in ABST method.
Simultaneous 8,10- gingerol and 6- zingiberol have more oxidation resistance than 6-gingerol in the researchs such as Swarnalatha discovery ginger,
These substances exist in 6-gingerol low content, play collaboration antioxidation.
Cortex Magnoliae Officinalis contains there are many ingredients such as chemical components, including phenols, alkaloids, volatile oil, flavonoids, polysaccharide,
Middle Magnolol and Honokiol is main active, at present both at home and abroad to the pharmacological research of Cortex Magnoliae Officinalis mainly wherein in magnolol and
The anti-oxidant of magnolol, antibacterial, it is antiviral, anti-inflammatory, antitumor the effects of, be directed to this year Cortex Magnoliae Officinalis polysaccharide the study found that thick
Plain polysaccharide has stronger ultra-oxygen anion free radical, DPPH free radical and ABTS+ Scavenging activity, higher Fe2+ chelating ability
And FRAP value, there is synergistic function from oxidation resistance is directed between different component in side reflection Magnolia cortex P.E.
Radix Angelicae Sinensis contains Ligustilide, and alias ligustilide is China's traditional Chinese medicine umbelliferae angelica volatile oil
Main active.Some researches show that extract for the steam distillation of Radix Angelicae Sinensis, and in the rhizoma ligustici of various concentration
The oxidation resistance of ester is studied, and should be theoretically that Ligustilide purity is higher, and oxidation resistance is better, but realizes knot
When fruit shows that Ligustilide content is minimum, oxidation resistance is most strong instead, when Ligustilide content is relatively high,
Its oxidation resistance is relatively weak, this shows the anti-oxidant energy that ingredient coexists to extract of Ligustilide between each extract
Power has played important synergistic function.Secondly, some researches show that Radix Angelicae Sinensis polysaccharide can significantly improve aging caused by D- galactolipin
SOD in model mice blood, CAT, the vigor of GSH-Px, reduce its blood plasma, in brain and liver homogenate LPO level, illustrate, Radix Angelicae Sinensis is more
Carbohydrate has good oxidation resistance.Radix Angelicae Sinensis polysaccharide and Ligustilide and other components have synergistic function.
Different groups of the independent any plant extracts of the above experiment conclusion and the existing studies have shown that synergistic effect
/, there is synergistic function, if above-mentioned 4 Plant Extracts compounded, between different component and difference is mentioned
It takes between object, also has synergy.
In conclusion the invention has the following advantages:
(1) preparation method of the composition with natural sun-prevention performance of the invention it is simple, conveniently, it is easy to operate, wherein adopting
Use supercritical CO2Natural plants are extracted, there is preferable extracting and developing efficiency, and has and integrates extracting and developing, concentration, whole
Body operating cost is low, no solvent residue, it is pollution-free, energy saving, easy to operate the advantages that.It is improved on extracting process,
Extraction yield is improved, more perfect bioactivity is saved.
(2) the part effective component in the composition produced by the present invention with natural sun-prevention performance is from numerous with sun-proof
It is screened in the natural plants of ability, avoids injuring to skin bring for the chemical suns such as organic synthesis, it can be by overcritical
Natural plant grease is obtained by extraction in CO2, can replace Synthetic Organic Chemistry sun-screening agent bring insecurity well.
(3) dendrobium candidum plays relatively good in performance of keeping humidity invention, and ginger is in the skin cares side such as moisturizing, antibacterial anti-inflammatory, anti-oxidant
The effect in face is fine, and polysaccharide is oxidation resistant main component in Radix Angelicae Sinensis, has stronger removing to hydroxy radical and oxygen radical
Effect, while polysaccharide has good moisture-keeping function again, and the magnolol in Cortex Magnoliae Officinalis is in addition to can be anti-oxidant, anti-aging, it is sun-proof outside,
Its significant effect in terms of anti-inflammatory.Therefore while considering sun-proof, the compounding discovery of 4 Plant Extracts is not adding
In the case where adding excessive moisturizer, moistening effect is preferable, and when not adding anti-sensitizer, antiallergic anti-inflammatory effects are relatively good, is not adding
In the case of adding preservative agent, there is certain anti-corrosion effect, therefore the formula of 4 kinds of extracts, not only on sun-proof result, at it
He can also have an unexpected effect at aspect, play green of the invention, inherent advantage.
(4) the composition produced by the present invention with natural sun-prevention performance on SPF preferably has higher
Sun-proof ability.Using sunscreen product obtained by natural sun-screening agents, the sense of human body skin is good, and using effect is good.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
A kind of preparation method of the composition with natural sun-prevention performance, comprising the following steps:
(1) part water, glycerol, allantoin and Carbopol being first heated to 90 DEG C in advance, heat preservation 40min is sterilized,
After be cooled to 85 DEG C of remaining glycerol of addition, allantoin and Carbopol, stir, heat preservation transparent to material dissolution
It is spare；A phase raw material includes 81 parts and 0.1 part of Carbopol of water according to mass parts；
(2) B phase raw material is heated to 88 DEG C, be uniformly mixed, B phase raw material includes: including stearic acid according to mass parts
1 part of glyceride, 1 part of cetostearyl alcohol olive oleate；
(3) uniformly mixed B phase raw material is poured slowly into A phase raw material, is stirred while adding, 180 turns of mixing speed/
Min, 75 DEG C of temperature；
(4) above-mentioned uniformly mixed raw material is subjected to emulsifying, homogeneous speed 3000 turns/min, homogenizing time 2min,
75 DEG C of temperature；
(5) above-mentioned material is cooled down while stirring, when temperature is down to 40 DEG C, the material after emulsification is added in C phase raw material
In stir evenly, 150 turns/min of mixing speed；C phase raw material includes 0.1 part of triethanolamine, dendrobium candidum extraction according to mass parts
0.3 part of object, 1.3 parts of ginger extract, 1.2 parts of Magnolia cortex P.E, 3 parts of angelica extract.
Wherein, the extraction conditions of dendrobium candidum extract are as follows: pressure 12MPa, 49 DEG C of temperature, CO2Flow 38L/h；Ginger mentions
Take the extraction conditions of object are as follows: pressure 20MPa, 40 DEG C of temperature, CO2Flow 30L/h；The extraction conditions of Magnolia cortex P.E are as follows: pressure
22MPa, 46 DEG C of temperature, CO2Flow 33L/h；The extraction conditions of angelica extract are as follows: pressure 30MPa, 53 DEG C of temperature, CO2Flow
32L/h。
Embodiment 2
A kind of preparation method of the composition with natural sun-prevention performance, comprising the following steps:
(1) part water, glycerol, allantoin and Carbopol are first heated to 80 DEG C in advance, heat preservation 250min is killed
Bacterium, after be cooled to 75 DEG C of remaining glycerol of addition, allantoin and Carbopol, stir transparent to material dissolution, protect
Warm standby is used；A phase raw material includes 79 parts and 0.2 part of Carbopol of water according to mass parts；
(2) B phase raw material is heated to 80 DEG C, be uniformly mixed, B phase raw material includes: PEG-100 tristearin according to mass parts
1.5 parts of the smooth olive oleate of 1.5 parts of acid esters, sorb, 2.5 parts of caprylic/capric triglyceride, 0.2 part of cetostearyl alcohol, cera alba
0.5 part
(3) uniformly mixed B phase raw material is poured slowly into A phase raw material, is stirred while adding, 220 turns of mixing speed/
Min, 85 DEG C of temperature；
(4) above-mentioned uniformly mixed raw material is subjected to emulsifying, homogeneous speed 4500 turns/min, homogenizing time 2min,
83 DEG C of temperature；
(5) above-mentioned material is cooled down while stirring, when temperature is down to 50 DEG C, the material after emulsification is added in C phase raw material
In stir evenly, 200 turns/min of mixing speed；C phase raw material includes 0.2 part of triethanolamine, dendrobium candidum extraction according to mass parts
0.7 part of object, 1.8 parts of ginger extract, 1.9 parts of Magnolia cortex P.E, 2.2 parts of angelica extract.
Wherein, the extraction conditions of dendrobium candidum extract are as follows: pressure 17MPa, 52 DEG C of temperature, CO2Flow 46L/h；Ginger mentions
Take the extraction conditions of object are as follows: pressure 30MPa, temperature 60 C, CO2Flow 30L/h；The extraction conditions of Magnolia cortex P.E are as follows: pressure
21MPa, 35 DEG C of temperature, CO2Flow 34L/h；The extraction conditions of angelica extract are as follows: pressure 20MPa, 40 DEG C of temperature, CO2Flow
3L/h。
Embodiment 3
A kind of preparation method of the composition with natural sun-prevention performance, comprising the following steps:
(1) part water, glycerol, allantoin and Carbopol being first heated to 87 DEG C in advance, heat preservation 28min is sterilized,
After be cooled to 80 DEG C of remaining glycerol of addition, allantoin and Carbopol, stir, heat preservation transparent to material dissolution
It is spare；A phase raw material includes 78 parts and 0.18 part of Carbopol of water according to mass parts；
(2) B phase raw material is heated to 90 DEG C, be uniformly mixed, B phase raw material includes: glycerol stearate according to mass parts
It is 0.5 part of ester, 1 part of PEG-100 stearate, 0.5 part of cetostearyl alcohol olive oleate, 0.5 part of the smooth olive oleate of sorb, pungent
2 parts of acid/Triglyceride DDD；
(3) uniformly mixed B phase raw material is poured slowly into A phase raw material, is stirred while adding, 190 turns of mixing speed/
Min, 79 DEG C of temperature；
(4) above-mentioned uniformly mixed raw material is subjected to emulsifying, homogeneous speed 3500 turns/min, homogenizing time 3min,
82 DEG C of temperature；
(5) above-mentioned material is cooled down while stirring, when temperature is down to 48 DEG C, the material after emulsification is added in C phase raw material
In stir evenly, 160 turns/min of mixing speed；C phase raw material includes 0.15 part of triethanolamine, dendrobium candidum extraction according to mass parts
0.6 part of object, 2 parts of ginger extract, 1 part of Magnolia cortex P.E, 2. part 1 of angelica extract, 0.25 part of silica.
Wherein, the extraction conditions of dendrobium candidum extract are as follows: pressure 17MPa, 55 DEG C of temperature, CO2Flow 32L/h；Ginger mentions
Take the extraction conditions of object are as follows: pressure 25MPa, 55 DEG C of temperature, CO2Flow 35L/h；The extraction conditions of Magnolia cortex P.E are as follows: pressure
22MPa, 46 DEG C of temperature, CO2Flow 42L/h；The extraction conditions of angelica extract are as follows: pressure 30MPa, temperature 60 C, CO2Flow
50L/h。
Embodiment 4
A kind of preparation method of the composition with natural sun-prevention performance, comprising the following steps:
(1) part water, glycerol, allantoin and Carbopol being first heated to 82 DEG C in advance, heat preservation 33min is sterilized,
After be cooled to 82 DEG C of remaining glycerol of addition, allantoin and Carbopol, stir, heat preservation transparent to material dissolution
It is spare；A phase raw material includes 75 parts and 0.13 part of Carbopol of water according to mass parts；
(2) B phase raw material is heated to 88 DEG C, be uniformly mixed, B phase raw material includes: glycerol stearate according to mass parts
1.1 parts of ester, 0.2 part of cetostearyl alcohol olive oleate, 0.8 part of the smooth olive oleate of sorb, 4 parts of caprylic/capric triglyceride,
4 parts of Butyrospermum parkii fruit rouge, 1.7 parts of PEG-8 dimethyl silicone polymer；
(3) uniformly mixed B phase raw material is poured slowly into A phase raw material, is stirred while adding, 200 turns of mixing speed/
Min, 75 DEG C of temperature；
(4) above-mentioned uniformly mixed raw material is subjected to emulsifying, homogeneous speed 4000 turns/min, homogenizing time 2min,
8 DEG C of temperature；
(5) above-mentioned material is cooled down while stirring, when temperature is down to 50 DEG C, the material after emulsification is added in C phase raw material
In stir evenly, 180 turns/min of mixing speed；C phase raw material includes 0.18 part of triethanolamine, dendrobium candidum extraction according to mass parts
0.8 part of object, 1 part of ginger extract, 2 parts of Magnolia cortex P.E, 3 parts of angelica extract, 0.4 part of silica.
Wherein, the extraction conditions of dendrobium candidum extract are as follows: pressure 15MPa, temperature 50 C, CO2Flow 30L/h；Ginger mentions
Take the extraction conditions of object are as follows: pressure 27MPa, 48 DEG C of temperature, CO2Flow 44L/h；The extraction conditions of Magnolia cortex P.E are as follows: pressure
27MPa, 40 DEG C of temperature, CO2Flow 40L/h；The extraction conditions of angelica extract are as follows: pressure 25MPa, 55 DEG C of temperature, CO2Flow
38L/h。
Embodiment 5
A kind of preparation method of the composition with natural sun-prevention performance, comprising the following steps:
(1) part water, glycerol, allantoin and Carbopol being first heated to 86 DEG C in advance, heat preservation 36min is sterilized,
After be cooled to 82 DEG C of remaining glycerol of addition, allantoin and Carbopol, stir, heat preservation transparent to material dissolution
It is spare；A phase raw material includes 84.24 parts and 0.2 part of Carbopol of water according to mass parts；
(2) B phase raw material is heated to 90 DEG C, be uniformly mixed, B phase raw material includes: glycerol stearate according to mass parts
0.2 part of ester, 1.2 parts of PEG-100 stearate, 0.3 part of cetostearyl alcohol olive oleate, 1.1 parts of the smooth olive oleate of sorb,
Include 0.5 part of cetostearyl alcohol, 1 part of cera alba, 2 parts of Butyrospermum parkii fruit rouge, 1 part of PEG-8 dimethyl silicone polymer；
(3) uniformly mixed B phase raw material is poured slowly into A phase raw material, is stirred while adding, 210 turns of mixing speed/
Min, 81 DEG C of temperature；
(4) above-mentioned uniformly mixed raw material is subjected to emulsifying, homogeneous speed 3000 turns/min, homogenizing time 3min,
85 DEG C of temperature；
(5) above-mentioned material is cooled down while stirring, when temperature is down to 40 DEG C, the material after emulsification is added in C phase raw material
In stir evenly, 190 turns/min of mixing speed；C phase raw material includes 0.13 part of triethanolamine, dendrobium candidum extraction according to mass parts
0.7 part of object, 1 part of ginger extract, 1.5 parts of Magnolia cortex P.E, 2.4 parts of angelica extract.
Wherein, the extraction conditions of dendrobium candidum extract are as follows: pressure 20MPa, temperature 60 C, CO2Flow 50L/h；Ginger mentions
Take the extraction conditions of object are as follows: pressure 22MPa, 43 DEG C of temperature, CO2Flow 38L/h；The extraction conditions of Magnolia cortex P.E are as follows: pressure
30MPa, temperature 50 C, CO2Flow 50L/h；The extraction conditions of angelica extract are as follows: pressure 27MPa, 43 DEG C of temperature, CO2Flow
45L/h。
Embodiment 6
A kind of preparation method of the composition with natural sun-prevention performance, comprising the following steps:
(1) part water, glycerol, allantoin and Carbopol being first heated to 81 DEG C in advance, heat preservation 35min is sterilized,
After be cooled to 85 DEG C of remaining glycerol of addition, allantoin and Carbopol, stir, heat preservation transparent to material dissolution
It is spare；A phase raw material includes 69.95 parts and 0.1 part of Carbopol of water according to mass parts；
(2) B phase raw material is heated to 80 DEG C, be uniformly mixed, B phase raw material includes: glycerol stearate according to mass parts
1.5 parts of ester, 1.5 parts of PEG-100 stearate, 1.5 parts of the smooth olive oleate of sorb, 0.4 part of cetostearyl alcohol, cera alba 0.7
Part, 3 parts of Butyrospermum parkii fruit rouge, 2 parts of PEG-8 dimethyl silicone polymer；
(3) uniformly mixed B phase raw material is poured slowly into A phase raw material, is stirred while adding, 220 turns of mixing speed/
Min, 72 DEG C of temperature；
(4) above-mentioned uniformly mixed raw material is subjected to emulsifying, homogeneous speed 5000 turns/min, homogenizing time 2min,
75 DEG C of temperature；
(5) above-mentioned material is cooled down while stirring, when temperature is down to 40 DEG C, the material after emulsification is added in C phase raw material
In stir evenly, 160 turns/min of mixing speed；C phase raw material includes 0.12 part of triethanolamine, dendrobium candidum extraction according to mass parts
0.9 part of object, 1.2 parts of ginger extract, 1.4 parts of Magnolia cortex P.E, 2 parts of angelica extract, 0.2 part of silica.
Wherein, the extraction conditions of dendrobium candidum extract are as follows: pressure 10MPa, 40 DEG C of temperature, CO2Flow 40L/h；Ginger mentions
Take the extraction conditions of object are as follows: pressure 28MPa, 58 DEG C of temperature, CO2Flow 49L/h；The extraction conditions of Magnolia cortex P.E are as follows: pressure
20MPa, 30 DEG C of temperature, CO2Flow 30L/h；The extraction conditions of angelica extract are as follows: pressure 28MPa, 48 DEG C of temperature, CO2 flow
32L/h。
Dendrobium candidum extract, ginger extract, Magnolia cortex P.E and angelica extract in the present invention are all made of overcritical
CO2Abstraction technique obtains.Supercritical CO2Abstraction technique extracts dendrobium candidum, ginger, Cortex Magnoliae Officinalis, the key component of Radix Angelicae Sinensis, right
Its plant extracts is measured ultraviolet scanning atlas, selects suitable absorption peak range and determines preferable extracted form natural plant
Object is optimal natural plant extracts under maximum absorption peak.According to the plant extracts of targeted specific peaks, selection is closed
Suitable concentration is compounded, to prepare the composition with natural sun-prevention ability.According to sunscreen composition obtained, it is added to institute
Have in the sunscreen product of preparation, forms the multifunctional natural sunscreen product that not only there is sun-screening function but also have both skin effect.
As shown in table 1, dendrobium candidum, ginger, Cortex Magnoliae Officinalis, Radix Angelicae Sinensis orthogonal experiments are obtained by orthogonal design table, then sieved
Best extraction process is selected, referring to table 2- table 5.
1 supercritical CO of table2Extract dendrobium candidum, ginger, Cortex Magnoliae Officinalis, Radix Angelicae Sinensis orthogonal array
2 supercritical CO of table2Extract dendrobium candidum optimised process
3 supercritical CO of table2Extract ginger optimised process
4 supercritical CO of table2Extract Cortex Magnoliae Officinalis optimised process
5 supercritical CO of table2Extract Radix Angelicae Sinensis optimised process
To the extract of above-mentioned extraction, precision is weighed in right amount respectively, and ethyl alcohol dissolution, being diluted to concentration is 10-40 μ g/ml's
Solution is used as sample, and quartz colorimetric utensil 1cm is swept within the scope of wavelength 280-400nm according to UV-VIS spectrophotometry
Face records and saves surface sweeping map, is handled with UVPC39 software the scanning spectra of preservation, and blank control is ethyl alcohol, sun
Property control be butyl dimethoxydibenzoylmethane (UVA sun-screening agent), 4 methyl benzylidene camphor (UVB sun-screening agent), 2- hydroxyl
Base -4- methoxy benzophenone (all band sun-screening agent).
(ε is dielectric constant to the ε value of each Plant Extracts of table 6, the dielectric constant at ultraviolet absorption peak maximum peak, is indicated
Ability of this substance to UV absorption)
Plant extracts relative mean values in table 7
As can be seen that angelica extract, ginger extract, Magnolia cortex P.E have resists UVB energy very well from table 6 and table 7
Power, dendrobium candidum extract and angelica extract have resists UVA ability very well, dendrobium candidum extract and angelica extract tool
Have and resists all band ability well.
In reference " cosmetics safety technical specification " chapter 8 human efficiency's evaluation test method, the sun-proof makeup of second part
Product SPF (spf value) measuring method and Part IV sunscreen cosmetic long wave ultraviolet protection index (PFA value) measurement side
Method is obtained by test, the SPF numerical intervals for the composition that the present invention is prepared are as follows: spf value between 20-30,
PA value is between 5-10, that is, between PA++-PA+++.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the composition with natural sun-prevention performance, which comprises the following steps:
(1) A phase raw material is subjected to sterilization processing, the rear temperature that adjusts to 75-85 DEG C, stir it is transparent to material dissolution,
It keeps the temperature spare；Wherein: A phase raw material includes 69.95-84.24 parts and Carbopol 0.1-0.2 parts of water according to mass parts；
(2) B phase raw material is heated to 80-90 DEG C, be uniformly mixed, in which: B phase raw material includes tristerin and PEG-
Gross mass part of one or both of 100 stearates, tristerin and PEG-100 stearate is 1-1.5 parts；B
Phase raw material further includes one or both of cetostearyl alcohol olive oleate and the smooth olive oleate of sorb, cetostearyl alcohol olive
Gross mass part of olive oleate and the smooth olive oleate of sorb is 1-1.5 parts；
(3) uniformly mixed B phase raw material is poured slowly into A phase raw material, is stirred while adding, 75-85 DEG C of temperature；
(4) above-mentioned uniformly mixed raw material is subjected to emulsifying, 75-85 DEG C of temperature；
(5) above-mentioned material is cooled down while stirring, when temperature is down to 40-50 DEG C, C phase raw material is added in the material after emulsification
It stirs evenly；Wherein: C phase raw material according to mass parts include triethanolamine 0.1-0.2 part 0,0.5-1 parts of dendrobium candidum extract,
1-2 parts of ginger extract, 1-2 parts of Magnolia cortex P.E, 2-3 parts of angelica extract.
2. the preparation method of the composition according to claim 1 with natural sun-prevention performance, which is characterized in that in (1)
In, A phase raw material further includes 3-6 mass parts glycerol and 0.05-0.1 mass parts allantoin, first by part water, glycerol, allantoin and
Carbopol is heated to 80-90 DEG C in advance, and heat preservation 25-40min is sterilized, after to be cooled to 75-85 DEG C of addition remaining sweet
Oil, allantoin and Carbopol, stir transparent to material dissolution, keep the temperature spare.
3. the preparation method of the composition according to claim 1 with natural sun-prevention performance, which is characterized in that in (2)
In, B phase raw material further includes caprylic/capric triglyceride, and the mass parts of the caprylic/capric triglyceride are 2-4 parts.
4. the preparation method of the composition according to claim 1 with natural sun-prevention performance, which is characterized in that in (2)
In, B phase raw material further includes 0.2-0.5 parts of cetostearyl alcohol, 0.5-1 parts of cera alba according to mass parts.
5. the preparation method of the composition according to claim 1 with natural sun-prevention performance, which is characterized in that in (2)
In, B phase raw material further includes 2-4 parts of Butyrospermum parkii fruit rouge, 1-2 parts of PEG-8 dimethyl silicone polymer according to mass parts.
6. the preparation method of the composition according to claim 1 with natural sun-prevention performance, which is characterized in that in (3)
In, mixing speed 180-220 turns/min；In (5), mixing speed 150-200 turns/min.
7. the preparation method of the composition according to claim 1 with natural sun-prevention performance, which is characterized in that in (4)
In, homogeneous speed 3000-5000 turns/min, homogenizing time 2-3min.
8. the preparation method of the composition according to claim 1 with natural sun-prevention performance, which is characterized in that in (5)
In, C phase raw material further includes 0.2-0.4 parts of silica according to mass parts.
9. the preparation method of the composition according to claim 1 with natural sun-prevention performance, which is characterized in that C is added
After phase raw material, when being cooled to 30-40 DEG C, essence 0.01-0.05 parts, 0.1-0.6 parts of preservative, mixing speed 150-200 is added
Turn/min, mixing time 20-30min, rear to stop stirring, that is, preparing terminates.
10. the preparation method of -9 described in any item compositions with natural sun-prevention performance, feature exist according to claim 1
In the extraction conditions of dendrobium candidum extract are as follows: pressure 10-20MPa, 40-60 DEG C of temperature, CO2Flow 30-50L/h；Ginger is extracted
The extraction conditions of object are as follows: pressure 20-30MPa, 40-60 DEG C of temperature, CO2Flow 30-50L/h；The extraction conditions of Magnolia cortex P.E
Are as follows: pressure 20-30MPa, 30-50 DEG C of temperature, CO2Flow 30-50L/h；The extraction conditions of angelica extract are as follows: pressure 20-
30MPa, 40-60 DEG C of temperature, CO2Flow 30-50L/h.
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