CN110179684A - It is a kind of can efficient absorption natural astaxanthin eye cream and preparation method thereof - Google Patents
It is a kind of can efficient absorption natural astaxanthin eye cream and preparation method thereof Download PDFInfo
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- CN110179684A CN110179684A CN201910592257.3A CN201910592257A CN110179684A CN 110179684 A CN110179684 A CN 110179684A CN 201910592257 A CN201910592257 A CN 201910592257A CN 110179684 A CN110179684 A CN 110179684A
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
- A61K8/068—Microemulsions
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/35—Ketones, e.g. benzophenone
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/37—Esters of carboxylic acids
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/67—Vitamins
- A61K8/678—Tocopherol, i.e. vitamin E
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- 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
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- A61Q19/00—Preparations for care of the skin
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Abstract
The present invention provide it is a kind of can efficient absorption astaxanthin eye cream, be that the free state astaxanthin after being heat-treated use to prepare as raw material；Free state astaxanthin after being wherein heat-treated is that astaxanthin is first extracted from raw material with solvent extraction method or supercritical fluid extraction, is then handled by enzymatic hydrolysis or method for saponification, and processing product is finally again through dicyandiamide solution heat treatment preparation.Astaxanthin eye cream of the invention can effectively remove free radical, to delay eye part skin aging, smooth away wrinkles and microgroove；Secondly, the astaxanthin in eye cream can effectively penetrate blood-retina barrier, the oxidation of retina and the damage of photosensory cell can be effectively prevented.And product storage-stable of the invention is strong, meets the shelf life needs of product, and it is most important to exploitation astaxanthin eye cream product.
Description
Technical field
The invention belongs to technical field of cosmetic preparation, and in particular to it is a kind of can efficient absorption natural astaxanthin eye cream and
Preparation method.
Background technique
Eye cream is primarily used to protection circumference of eyes skin.It is well known that the skin of circumference of eyes is Whole Body skin
Most thin in skin tissue, thickness is only 0.33~0.36 millimeter, especially soft and fine slim, very fragile, needs to double to maintain.
Astaxanthin has different physiological roles, referred to as " super antioxygen as a kind of fat soluble carotenoids substance
Agent ".Studies have shown that the oxidation resistance of astaxanthin is 100 times of vitamin E, it is strong that brilliant oxidation resistance assigns it
The effect of big removing free radical and anti-aging, thus be widely used in functional form cosmetics.And astaxanthin is as only
One can penetrate the carotenoid of blood-retina barrier, be of great significance to visual fatigue and protection eyes are alleviated.Therefore, will
Astaxanthin is added in eye cream as efficacy factor, will widen the application field of astaxanthin with important to care eye health
Meaning.
However, astaxanthin has the defects such as dissolubility is poor, stability is poor, bioavailability is low, seriously limit its application.
Summary of the invention
The present invention provide it is a kind of can efficient absorption astaxanthin eye cream, free radical can be effectively removed, to delay eye
Portion's skin aging, smoothes away wrinkles and microgroove；Secondly, the astaxanthin in eye cream can effectively penetrate blood-retina barrier, it can be effectively
Prevent the oxidation of retina and the damage of photosensory cell.And product storage-stable of the invention is strong, meets the shelf of product
Phase needs, most important to exploitation astaxanthin eye cream product.
Astaxanthin eye cream of the invention is that the free state astaxanthin after heat treatment is used to prepare as raw material；Wherein at heat
Free state astaxanthin after reason is that astaxanthin is first extracted from raw material with solvent extraction method or supercritical fluid extraction, is then led to
It crosses enzymatic hydrolysis or method for saponification is handled, processing product is finally again through dicyandiamide solution heat treatment preparation；
The described dicyandiamide solution heat treatment is that will be added to by the astaxanthin that enzymatic hydrolysis or method for saponification are handled can not
It fires in low boiling point solvent, 0.5~50h is handled under the conditions of temperature is 40~90 DEG C；After remove organic solvent, obtain hot place
Free state astaxanthin after reason；
The non-combustible low boiling point solvent is any one or more of methylene chloride, dimethyl sulfoxide or ethyl acetate；
Preferably, also adding powdered I-TiO in heat treatment process2Catalyst as heat treatment process.
The wherein solvent extraction method, wherein solvent be dehydrated alcohol, acetone, ethyl acetate, methylene chloride or just oneself
Any one or more of alkane.
The raw material is haematococcus pluvialis or red phaffia rhodozyma.
Astaxanthin eye cream of the invention, it is a kind of specific the preparation method is as follows:
1) free state astaxanthin nanometer micro-emulsion is prepared:
Free state astaxanthin is added in carrier oil in the ratio of mass fraction 0.005~5%, and is stirred to completely molten
Solution forms free state astaxanthin oil solution；Then oil-soluble inhibitor, emulsifier are added into obtained oil solution and/or helps
Emulsifier, uniform stirring；Dissolvent residual is removed after stirring, is prepared rich in free state astaxanthin nanometer micro-emulsion；
Wherein the carrier oil is the mixture of one or more of straight-chain fatty acid ester and fatty glyceride.
The oil-soluble inhibitor is tocopherol, tocopherol acetate, ubiquinone, gallate, butylhydroxy fennel
One or more of fragrant ether, dibutyl hydroxy toluene and carnosic acid；Matter of the oil-soluble inhibitor in basic oil solution
Measuring volume fraction is 0.0005%~1%；
The emulsifier is tween, sapn, PLURONICS F87, Emulsifier EL-60, soybean lecithin, lecithin, gathers
One or more of vinyl alcohol or poly lactic-co-glycolic acid；
The assistant for emulsifying agent be one of ethyl alcohol, 1,2- propylene glycol, 1,3- propylene glycol, glycerine or polyethylene glycol or
It is several；
2) prepared by water phase:
The weight percent of each ingredient of water phase is as follows: 0.1~2% stabilizer, 0.5~15% cosolvent, 0.001~3%
Water soluble antioxidant, surplus are deionized water；
The stabilizer be xanthan gum, lactalbumin, casein sodium, gelatin, polylysine, chitosan, albumin,
One or more of Arabic gum, sodium alginate, hydroxymethyl cellulose.
The cosolvent is one of ethyl alcohol, 1,2- propylene glycol, 1,3- propylene glycol, glycerine or polyethylene glycol or several
Kind,
The water soluble antioxidant is tea polyphenols, ascorbic acid or its sodium salt, in ethylenediamine tetra-acetic acid or its sodium salt
One or more.
It is furthermore preferred that water phase wherein also dissolved with weight fraction be 0.01~1% preservative and 0~2% fruit essence,
The preservative is one or more of ethyl hydroxy benzoate, Nipasol or butyl hydroxybenzoate.
3) it mixes homogeneous: the aqueous phase solution of the free state astaxanthin nanometer micro-emulsion of step 1) preparation and step 2) is distinguished
40~80 DEG C are preheating to, then astaxanthin nanometer micro-emulsion is added in water phase according to the ratio of 1:0.3~4, side edged stirs
It mixes；It is uniformly mixed and is placed on 5~30min of emulsifying in vacuum emulsifying machine, 40~80 DEG C of process control temp, be then cooled to
10~35 DEG C of completion preparations.
Prepared by the present invention can efficient absorption astaxanthin eye cream, have the following advantages that.
1, the present invention prepared by can efficient absorption astaxanthin eye cream, using the free state astaxanthin of heat treatment as raw material,
Nanoscale microemulsion system is devised, free state astaxanthin be absorbed and utilized can effectively by skin tissue, and then can be in skin
Organization internal effectively plays anti-oxidant and reparation effect；Show in 24 hours of astaxanthin in product of the present invention through in vitro test
Transdermal absorption factor is accumulated 65% or more, and remains in the astaxanthin of skin surface, can be effective against outer grenz rays and freedom
Damage of the base to eye skin, achievees the effect that dual care.
2, the present invention prepared by can efficient absorption astaxanthin eye cream shelf life stability it is excellent, accelerated storage test
Show in its 2 year storage period, total astaxanthin retention rate maintains 80% or more in lipstick, can long term storage, sufficiently meet commodity
Shelf life demand.
3, the present invention prepared by can efficient absorption astaxanthin eye cream to eye part skin hydrauture, drying, coarse, bullet
Property, compact, wrinkle have significantly improve effect.
Specific embodiment
The present invention selects the free state astaxanthin after heat treatment as raw material, designs in combination with astaxanthin microemulsion system,
The absorptivity of astaxanthin is improved in terms of molecular structure and carrier systems two, so that the effect of giving full play to astaxanthin, improves
Its shelf life stability.
The present invention is described in detail below with reference to embodiment.
Embodiment 1
The preparation method of astaxanthin eye cream, comprising the following steps:
1) prepared by free state astaxanthin:
Using haematococcus pluvialis as the biological raw material of preparation esterification of astaxanthin, the haematococcus pluvialis powder of 1kg is weighed, is added 10
The dehydrated alcohol of times material quality (W/V) extracts 2 times repeatedly, extracts 1h every time, merges leaching liquor, then leaching liquor is through depressurizing
Concentration removal solvent, obtains crude extract；Then the potassium hydroxide solution that the mass concentration of 30 times of volumes is 2% is added in crude extract
In, saponification is carried out in 4 DEG C and inflated with nitrogen under the conditions of, after reaction by reaction system as standing 2h under the conditions of -2 DEG C,
Then it filters, collects the purplish red color substance that crystallization is precipitated to get the free state astaxanthin of purification is arrived.
2) free state astaxanthin is heat-treated:
It weighs and is dissolved in the astaxanthin that step 1) obtains in dichloromethane solution by 2% bulking value score (g/ml),
Then continuous heat 4h under conditions of closed nitrogen charging, 70 DEG C removes organic solvent through being concentrated under reduced pressure after terminating, obtains hot place
Free state astaxanthin after reason.
3) free state astaxanthin micro emulsion is prepared:
Free state astaxanthin after heat treatment is added in ethyl acetate in the ratio of mass fraction 1%, and is stirred
Free state astaxanthin ethyl acetate solution is formed to being completely dissolved；Then it is 0.01% that quality volume fraction is successively added thereto
Vitamin E, 10% Tween 80 and 5% glycerine, uniform stirring；It is evaporated under the conditions of low-temp low-pressure after stirring de-
Except dissolvent residual, it is prepared rich in free state astaxanthin nanometer micro-emulsion；
4) prepared by water phase: prepare aqueous phase solution, make xanthan gum wherein containing weight fraction 0.2%, 10% it is anhydrous
Ethyl alcohol (being wherein 0.05% ethyl hydroxy benzoate and 0.1% flavoring apple essence containing weight fraction), 0.01% tea polyphenols.Configuration
Make to disperse each component in deionized water, be stirred well to and be completely dissolved, obtains water phase.
5) mix homogeneous: aqueous phase solution by the free state astaxanthin nanometer micro-emulsion of step 3) preparation and 4) preheats respectively
To 60 DEG C, then astaxanthin nanometer micro-emulsion is added in water phase according to the ratio of 1:1, process is stirring while adding.Mixing is equal
Even to be placed in vacuum emulsifying machine, emulsifying 15min, is cooled to 25 DEG C then to get can be efficient by 75 DEG C of process control temp
The astaxanthin eye cream of absorption.
Embodiment 2
A kind of preparation method of astaxanthin eye cream, comprising the following steps:
1) prepared by free state astaxanthin: using haematococcus pluvialis as the biological raw material of preparation esterification of astaxanthin, weighing 100g
Haematococcus pluvialis powder is added the ethyl acetate extraction 4h of 20 times of material qualities (W/V), leaching liquor is collected by filtration, then leaching liquor
It is concentrated under reduced pressure, removes solvent, obtain crude extract.Then to the Tween 80 of 1 times of quality, then emulsifying is added fatty
The phosphate buffer of enzyme, the dosage of enzyme are the total astaxanthin of 10U/ μ g, and enzymatic hydrolysis condition is 40 DEG C, pH5.5, enzymolysis time 12h.Enzyme
After solution, ethyl acetate is added into system, until demulsification, collects oily phase, be concentrated under reduced pressure, obtain free state astaxanthin；
2) free state astaxanthin is heat-treated:
It weighs and is dissolved in the astaxanthin that step 1) obtains in ethyl acetate solution by 3% bulking value score, add simultaneously
Enter the powdered I-TiO that bulking value score is 6%2, then continuous heat 2h under conditions of closed nitrogen charging, 60 DEG C, is tied
Powdered I-TiO is recovered by filtration after beam2, for solution through reduced pressure removing organic solvent, the free state shrimp after being heat-treated is green
Element.
3) prepare free state astaxanthin nanometer micro-emulsion: the free state astaxanthin after the heat treatment that step 2) is obtained is by matter
The ratio of amount score 0.5% is added in ethyl oleate, and stirs that form free state astaxanthin oil acetoacetic ester molten to being completely dissolved
Liquid；Then successively thereto be added quality volume fraction be 0.01% Co-Q10,10% Tween 80 and 5% glycerine,
Uniform stirring；Evaporation removes dissolvent residual under the conditions of low-temp low-pressure after stirring, is prepared rich in free state astaxanthin
Nanometer micro-emulsion；
4) prepared by water phase: preparing aqueous phase solution, makes glycerine (its of gelatin wherein containing weight fraction 1%, 15%
In containing weight fraction be 0.05% Nipasol and 0.1% mango essence), 0.02% ascorbic acid.Configuration make by
Each component is scattered in deionized water, is stirred well to and is completely dissolved, and water phase is obtained.
5) mix homogeneous: aqueous phase solution by the free state astaxanthin nanometer micro-emulsion of step 3) preparation and 4) preheats respectively
To 65 DEG C, then astaxanthin nanometer micro-emulsion is added in water phase according to the ratio of 1:1.5, process is stirring while adding.Mixing
It is uniformly placed in vacuum emulsifying machine, emulsifying 20min, 70 DEG C of process control temp, is cooled to 30 DEG C then to get can be high
Imitate the astaxanthin eye cream absorbed.
Embodiment 3
A kind of preparation method of astaxanthin eye cream, comprising the following steps:
1) prepared by free state astaxanthin: weigh red phaffia rhodozyma 100g, in the extraction kettle in 1L supercritical extraction unit,
The temperature of extraction kettle is set as 40 DEG C, and pressure is set as 30MPa, extractant CO2Flow set be 20L/h, the temperature of separation reactor I
Degree and pressure are respectively 35 DEG C and 10MPa, and the temperature of separation reactor I I is 40 DEG C, CO2The flow velocity of fluid is 30L/h, continuous dynamic
Extraction time is 3h, and extract is aperiodically released from separating still, collects and is stored in container, and extract is in kermesinus
Sticky mass obtains the crude extract rich in free state astaxanthin；Then the free state astaxanthin refined is chromatographed by column；
2) free state astaxanthin is heat-treated: being weighed and is dissolved in the astaxanthin that step 1) obtains by 8% bulking value score
In dimethyl sulfoxide solution, while the powdered I-TiO that bulking value score is 10% is added2, then in closed nitrogen charging, 70 DEG C
Under the conditions of continuous heat 2h, after powdered I-TiO is recovered by filtration2, solution is concentrated under reduced pressure, the trip after being heat-treated
Amorph astaxanthin.
3) it prepares free state astaxanthin nanometer micro-emulsion: free state astaxanthin is added in the ratio of mass fraction 0.1%
Into olive oil, and stir to being completely dissolved to form free state astaxanthin olive oil solution；Then quality is successively added thereto
Volume fraction be 0.01% vitamin E, 8% polysorbate85 and 5% ethyl alcohol, uniform stirring；It is low in low temperature after stirring
Evaporation removing dissolvent residual, is prepared rich in free state astaxanthin nanometer micro-emulsion under the conditions of pressure；
4) prepared by water phase: preparing aqueous phase solution, makes the poly- second two of chitosan wherein containing weight fraction 1%, 10%
Alcohol 400 (being wherein 0.05% Nipasol and 0.1% orange taste essence containing weight fraction), 0.04% ethylenediamine tetrem
Sour sodium.Configuration makes to disperse each component in deionized water, is stirred well to and is completely dissolved, obtains water phase.
5) mix homogeneous: aqueous phase solution by the free state astaxanthin nanometer micro-emulsion of step 3) preparation and 4) preheats respectively
To 70 DEG C, then astaxanthin nanometer micro-emulsion is added in water phase according to the ratio of 1:2, process is stirring while adding.Mixing is equal
Even to be placed in vacuum emulsifying machine, emulsifying 10min, is cooled to 20 DEG C then to get can be efficient by 75 DEG C of process control temp
The astaxanthin eye cream of absorption.
Comparative example 4
A kind of preparation method of astaxanthin eye cream, comprising the following steps:
1) prepared by free state astaxanthin: using haematococcus pluvialis as the biological raw material of preparation esterification of astaxanthin, weighing 1kg's
The dehydrated alcohol of 10 times of material qualities (W/V) is added in haematococcus pluvialis powder, extracts 2 times repeatedly, extracts 1h every time, merges extraction
Liquid, then leaching liquor is concentrated under reduced pressure, and is removed solvent, is obtained crude extract；Then the quality for 30 times of volumes being added in crude extract is dense
In the potassium hydroxide solution that degree is 2%, saponification is carried out under the conditions of 4 DEG C and inflated with nitrogen, after reaction by reaction system
It as 2h is stood under the conditions of -2 DEG C, then filters, it is green to get the free state shrimp to purification to collect the purplish red color substance that crystallization is precipitated
Element.
2) it prepares free state astaxanthin micro emulsion: the free state astaxanthin after heat treatment is added in the ratio of mass fraction 1%
It is added in ethyl acetate, and stirs to being completely dissolved to form free state astaxanthin ethyl acetate solution；Then successively thereto
Addition quality volume fraction be 0.01% vitamin E, 10% Tween 80 and 5% glycerine, uniform stirring；Stirring terminates
Evaporation removing dissolvent residual under the conditions of low-temp low-pressure afterwards, is prepared rich in free state astaxanthin nanometer micro-emulsion；
3) prepared by water phase: prepare aqueous phase solution, make xanthan gum wherein containing weight fraction 0.2%, 10% it is anhydrous
Ethyl alcohol (being wherein 0.05% ethyl hydroxy benzoate and 0.1% flavoring apple essence containing weight fraction), 0.01% tea polyphenols.Configuration
Make to disperse each component in deionized water, be stirred well to and be completely dissolved, obtains water phase.
4) mix homogeneous: aqueous phase solution by the free state astaxanthin nanometer micro-emulsion of step 3) preparation and 4) preheats respectively
To 60 DEG C, then astaxanthin nanometer micro-emulsion is added in water phase according to the ratio of 1:1, process is stirring while adding.Mixing is equal
Even to be placed in vacuum emulsifying machine, emulsifying 15min, is cooled to 25 DEG C then to get can be efficient by 75 DEG C of process control temp
The astaxanthin eye cream of absorption.
Embodiment 5 detects: the test of sun-proof and repair function
Test object is the eye cream sample of astaxanthin eye cream sample prepared by embodiment 1 and comparative example 4.
Healthy mice 6, quality (20 ± 2) Kunming g is chosen, half male and half female is randomly divided into 2 groups, every group 3.Respectively to small
Mouse prophylactically smears test sample and control sample, and every back 2 times/d, is smeared to 0.6mL, every monaural to 0.3mL altogether
4d.Mouse is horizontally fixed on brandreth and is placed in away from 6h is irradiated at ultraviolet lamp vertical range 10cm, skin lesion mouse model is caused.
Using mouse skin keratinization and decortication degree as evaluation index, back of mice change of skin situation is observed, analyzes sample to mouse
The protective effect of skin resistance ultraviolet injury.
Skin lesion mouse model is continued to irradiate after 40h ridge execution of breaking with ultraviolet light, weighs mouse quality, then take two ears respectively
And the round auricle and skin graft of back 9mm diameter, its quality of accurate weighing calculate ear index (ear index=auricle quality/mouse
Quality) and skin index (skin index=skin graft quality/mouse quality), analysis sample is to the ultraviolet inhibition work for shooting mouse oedema wounded
With.After taking back portion skin to be fixed for 24 hours with 10% formaldehyde, sealing sample is made.Sealing sample is placed in 10 times of microscopic observations
Skin configuration, the skin observed under 40 times of mirrors since the visual field clap the first picture, later every movement topmost
Scale 2mm bat takes one, and bat takes 5 Zhang Houyong microimage analysing systems to choose 5 points on every picture, measures its epidermis thickness
Degree, every picture measure 25 points altogether, are averaged and are denoted as epidermal thickness, and analysis sample makees the inhibition of mouse skin keratinization
With.Every picture takes 6 visuals field, counts fibroblast number in each visual field, is averaged and is denoted as each visual field corium into fibre
Tie up cell number.
Ultraviolet injury mouse ear index, skin index, epidermal thickness and fibroblast measurement result are shown in Table 1.
Table 1: ultraviolet injury mouse ear index, skin index, epidermal thickness and fibroblast
The result shows that applying mouse ear index, the skin index, epidermal thickness for using test sample after mouse is irradiated by ultraviolet light
Value is lower than painting comparative example sample, and fibroblast number is more than painting control sample in dermal tissue.Cause
This, above-mentioned test result shows to be remarkably improved astaxanthin eye cream to skin by being heat-treated free state astaxanthin
Protection and repair.
6 Detection of Stability of embodiment
The astaxanthin eye cream sample that embodiment 1, embodiment 2, embodiment 3 are prepared, in being protected from light guarantor under room temperature
Total astaxanthin retention rate therein is measured after depositing 30 days, and has seen whether precipitation, if layering, if has peculiar smell, with evaluation
The present invention prepares the stability of astaxanthin eye cream, and test result is as shown in table 2.
The retention rate calculation formula of total astaxanthin is as follows:
Retention rate (%)=C of total astaxanthin30/C0× 100%
Wherein, C0For content astaxanthin total in initial sample；C30Content astaxanthin in sample after being storage 30 days.
Table 2: stability test result
It can be seen from the result of table 2 in astaxanthin eye cream prepared by the present invention, astaxanthin has good stability.Meanwhile it making
Standby obtained astaxanthin eye cream stable system, no precipitation lamination, and without generating peculiar smell.
Finally it may be noted that the embodiment of the present invention is the preferable embodiment of the present invention, but embodiments of the present invention are simultaneously
Be not restricted to the described embodiments, it is other it is any without departing from the spirit and principles of the present invention made by change, modification,
Substitution, simplifies combination, is regarded as equivalent substitute mode, is included in protection scope of the present invention.
Claims (10)
1. a kind of astaxanthin eye cream, which is characterized in that the astaxanthin eye cream is made with the free state astaxanthin after heat treatment
For raw material preparation；Free state astaxanthin after being wherein heat-treated is first to use solvent extraction method or supercritical fluid extraction from original
Astaxanthin is extracted in material, is then handled by enzymatic hydrolysis or method for saponification, and processing product is finally heat-treated through dicyandiamide solution again
Preparation；
The described dicyandiamide solution heat treatment, be will be added to by the astaxanthin that enzymatic hydrolysis or method for saponification are handled it is non-combustible low
In boiling point solvent, 0.5~50h is handled under the conditions of temperature is 40~90 DEG C；After remove organic solvent, after obtaining heat treatment
Free state astaxanthin.
2. astaxanthin eye cream as described in claim 1, which is characterized in that the non-combustible low boiling point solvent is dichloromethane
Any one or more of alkane, dimethyl sulfoxide or ethyl acetate.
3. astaxanthin eye cream as described in claim 1, which is characterized in that also add powdered I-TiO in heat treatment process2Make
For the catalyst of heat treatment process.
4. astaxanthin eye cream as described in claim 1, which is characterized in that the solvent extraction method, wherein solvent is anhydrous
Any one or more of ethyl alcohol, acetone, ethyl acetate, methylene chloride or n-hexane.
5. astaxanthin eye cream as described in claim 1, which is characterized in that the raw material is haematococcus pluvialis or red Fife's ferment
It is female.
6. astaxanthin eye cream as described in claim 1, which is characterized in that the astaxanthin eye cream the preparation method is as follows:
1) free state astaxanthin nanometer micro-emulsion is prepared:
Free state astaxanthin is added in carrier oil, and stirs to being completely dissolved to form free state astaxanthin oil solution；Then
Oil-soluble inhibitor, emulsifier and/or assistant for emulsifying agent, uniform stirring are added into obtained oil solution；It is taken off after stirring
Except dissolvent residual, it is prepared rich in free state astaxanthin nanometer micro-emulsion；
2) prepared by water phase:
The weight percent of each ingredient of water phase is as follows: 0.1~2% stabilizer, 0.5~15% cosolvent, 0.001~3% water-soluble
Property antioxidant, surplus is deionized water；
3) it mixes homogeneous: the aqueous phase solution of the free state astaxanthin nanometer micro-emulsion of step 1) preparation and step 2) is preheated respectively
To 40~80 DEG C, then astaxanthin nanometer micro-emulsion is added in water phase according to the ratio of 1:0.3~4, it is stirring while adding；It is mixed
It closes and is uniformly placed on 5~30min of emulsifying in vacuum emulsifying machine, 40~80 DEG C of process control temp, then it is cooled to 10~
35 DEG C of completion preparations.
7. astaxanthin eye cream as claimed in claim 6, which is characterized in that described 1) in carrier oil be straight-chain fatty acid ester
With the mixture of one or more of fatty glyceride.
8. astaxanthin eye cream as claimed in claim 6, which is characterized in that described 1) in oil-soluble inhibitor make a living
It educates in phenol, tocopherol acetate, ubiquinone, gallate, butylated hydroxy anisole, dibutyl hydroxy toluene and carnosic acid
One or more；
The emulsifier is tween, sapn, PLURONICS F87, Emulsifier EL-60, soybean lecithin, lecithin, polyethylene
One or more of alcohol or poly lactic-co-glycolic acid；
The assistant for emulsifying agent is one of ethyl alcohol, 1,2- propylene glycol, 1,3- propylene glycol, glycerine or polyethylene glycol or several
Kind.
9. astaxanthin eye cream as claimed in claim 6, which is characterized in that described 2) described in stabilizer be xanthan gum,
Lactalbumin, casein sodium, gelatin, polylysine, chitosan, albumin, Arabic gum, sodium alginate, hydroxylmethyl cellulose
One or more of element；
The cosolvent is one or more of ethyl alcohol, 1,2-PD, 1,3-PD, glycerine or polyethylene glycol,
The water soluble antioxidant is tea polyphenols, ascorbic acid or its sodium salt, one in ethylenediamine tetra-acetic acid or its sodium salt
Kind is several.
10. astaxanthin eye cream as claimed in claim 6, which is characterized in that the water phase is wherein also dissolved with preservative and water
Fruity essence.
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| CN110179684B (en) | 2022-05-10 |
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