CN110179684B - Natural astaxanthin eye cream capable of being efficiently absorbed and preparation method thereof - Google Patents
Natural astaxanthin eye cream capable of being efficiently absorbed and preparation method thereof Download PDFInfo
- Publication number
- CN110179684B CN110179684B CN201910592257.3A CN201910592257A CN110179684B CN 110179684 B CN110179684 B CN 110179684B CN 201910592257 A CN201910592257 A CN 201910592257A CN 110179684 B CN110179684 B CN 110179684B
- Authority
- CN
- China
- Prior art keywords
- astaxanthin
- eye cream
- free
- heat treatment
- solvent
- 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.)
- Active
Links
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
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
- A61K8/068—Microemulsions
-
- 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
-
- 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
- A61K8/67—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
- A61K8/92—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
- 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
- A61Q19/005—Preparations for sensitive 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
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Dermatology (AREA)
- Chemical & Material Sciences (AREA)
- Emergency Medicine (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Dispersion Chemistry (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Medicinal Preparation (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention provides an astaxanthin eye cream capable of being efficiently absorbed, which is prepared by using free astaxanthin after heat treatment as a raw material; wherein the free astaxanthin after heat treatment is prepared by extracting astaxanthin from raw materials by solvent extraction method or supercritical fluid extraction method, treating by enzymolysis or saponification method, and heat treating the treated product by solvent system. The astaxanthin eye cream can effectively remove free radicals, so that the aging of eye skin is delayed, and wrinkles and fine lines are eliminated; second, astaxanthin in eye cream effectively penetrates the blood-retinal barrier and effectively prevents retinal oxidation and photoreceptor cell damage. The product of the invention has strong storage stability, meets the shelf life requirement of the product and is very important for developing astaxanthin eye cream products.
Description
Technical Field
The invention belongs to the technical field of cosmetic preparation, and particularly relates to natural astaxanthin eye cream capable of being efficiently absorbed and a preparation method thereof.
Background
The eye cream is mainly used for protecting skin around eyes. As is known, the skin around the eyes is the thinnest of the skin tissues of the whole body of a human body, the thickness is only 0.33-0.36 mm, and the skin is particularly soft, thin and fragile and needs to be maintained twice.
Astaxanthin, a fat-soluble carotenoid, has a variety of physiological functions and is called a "super antioxidant". Research shows that the antioxidant capacity of astaxanthin is 100 times that of vitamin E, and the excellent antioxidant capacity of astaxanthin endows the astaxanthin with strong effects of scavenging free radicals and delaying senescence, so that the astaxanthin is widely applied to functional cosmetics. And astaxanthin is used as the only carotenoid capable of penetrating through the blood-retina barrier, and has important significance for relieving asthenopia and protecting eyes. Therefore, the astaxanthin serving as an efficacy factor is added into the eye cream, and the eye cream has important significance for caring eye health and widening the application field of the astaxanthin.
However, astaxanthin has the defects of poor solubility, poor stability, low bioavailability and the like, and the application of astaxanthin is severely limited.
Disclosure of Invention
The invention provides the astaxanthin eye cream capable of being efficiently absorbed, which can effectively remove free radicals, thereby delaying the skin aging of eyes and eliminating wrinkles and fine lines; second, astaxanthin in eye cream effectively penetrates the blood-retinal barrier and effectively prevents retinal oxidation and photoreceptor cell damage. The product of the invention has strong storage stability, meets the shelf life requirement of the product and is very important for developing astaxanthin eye cream products.
The astaxanthin eye cream is prepared by using free astaxanthin after heat treatment as a raw material; wherein the heat-treated free astaxanthin is prepared by extracting astaxanthin from raw materials by solvent extraction method or supercritical fluid extraction method, treating by enzymolysis or saponification method, and heat-treating the treated product with solvent system;
the heat treatment of the solvent system is to add the astaxanthin treated by the enzymolysis or saponification method into the non-flammable low-boiling-point solvent and treat the astaxanthin for 0.5 to 50 hours at the temperature of 40 to 90 ℃; removing the organic solvent after the completion of the step to obtain the free astaxanthin after heat treatment;
the non-flammable low-boiling point solvent is any one or more of dichloromethane, dimethyl sulfoxide or ethyl acetate;
preferably, powdered I-TiO is also added during the heat treatment2As a catalyst for the heat treatment process.
The solvent extraction method comprises the step of extracting the solvent by using a solvent, wherein the solvent is any one or more of absolute ethyl alcohol, acetone, ethyl acetate, dichloromethane or normal hexane.
The raw material is haematococcus pluvialis or phaffia rhodozyma.
The astaxanthin eye cream has the specific preparation method as follows:
1) preparing free astaxanthin nano microemulsion:
adding free astaxanthin into carrier oil according to the mass fraction of 0.005-5%, and stirring until the free astaxanthin is completely dissolved to form a free astaxanthin oil solution; then adding an oil-soluble antioxidant, an emulsifier and/or an auxiliary emulsifier into the obtained oil solution, and uniformly stirring; removing solvent residues after stirring is finished, and preparing the free astaxanthin-rich nano microemulsion;
wherein the carrier oil is one or a mixture of more of linear chain fatty acid ester and fatty glyceride.
The oil-soluble antioxidant is one or more of tocopherol, tocopheryl acetate, coenzyme Q, gallate, butyl hydroxy anisole, dibutyl hydroxy toluene and carnosic acid; the mass volume fraction of the oil-soluble antioxidant in the base oil solution is 0.0005-1%;
the emulsifier is one or more of tween, span, poloxamer 188, polyoxyethylene castor oil, soybean phospholipid, lecithin, polyvinyl alcohol or polylactic acid-glycolic acid;
the auxiliary emulsifier is one or more of ethanol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol or polyethylene glycol;
2) preparation of an aqueous phase:
the water phase comprises the following components in percentage by weight: 0.1-2% of stabilizer, 0.5-15% of cosolvent, 0.001-3% of water-soluble antioxidant and the balance of deionized water;
the stabilizer is one or more of xanthan gum, lactalbumin, sodium caseinate, gelatin, polylysine, chitosan, albumin, acacia, sodium alginate and hydroxymethyl cellulose.
The cosolvent is one or more of ethanol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol or polyethylene glycol,
the water-soluble antioxidant is one or more of tea polyphenol, ascorbic acid or sodium salt thereof, and ethylene diamine tetraacetic acid or sodium salt thereof.
More preferably, the water phase also contains 0.01-1 wt% of preservative and 0-2 wt% of fruit essence, wherein the preservative is one or more of ethylparaben, propylparaben or butylparaben.
3) Mixing and homogenizing: preheating the free astaxanthin nano microemulsion prepared in the step 1) and the aqueous phase solution prepared in the step 2) to 40-80 ℃, and then adding the astaxanthin nano microemulsion into the aqueous phase according to the proportion of 1: 0.3-4 while stirring; after being uniformly mixed, the mixture is put into a vacuum emulsifying machine for homogenizing and emulsifying for 5-30 min, the temperature is controlled to be 40-80 ℃ in the process, and then the temperature is reduced to 10-35 ℃ to finish the preparation.
The astaxanthin eye cream capable of being efficiently absorbed, which is prepared by the invention, has the following advantages.
1. The astaxanthin eye cream capable of being efficiently absorbed, which is prepared by the invention, takes the heat-treated free astaxanthin as a raw material, and a nano-scale microemulsion system is designed, so that the free astaxanthin can be effectively absorbed and utilized by skin tissues, and further, the antioxidant and repairing effects can be effectively exerted in the skin tissues; in vitro tests show that the accumulated transdermal absorption rate of the astaxanthin in the product is more than 65% within 24 hours, and the astaxanthin remained on the surface of the skin can effectively resist the damage of external rays and free radicals to the eye skin, thereby achieving the effect of double care.
2. The astaxanthin eye cream capable of being efficiently absorbed has excellent shelf life stability, and accelerated storage tests show that the total astaxanthin retention rate in the lipstick is maintained to be more than 80% within two-year storage period, so that the astaxanthin eye cream can be stored for a long time, and the requirement of commodity shelf life is fully met.
3. The astaxanthin eye cream capable of being efficiently absorbed has obvious improvement effects on the hydration degree, dryness, roughness, elasticity, compactness and wrinkles of eye skin.
Detailed Description
The invention selects the free astaxanthin after heat treatment as a raw material, and simultaneously improves the absorption rate of the astaxanthin from two aspects of molecular structure and carrying system by combining the design of an astaxanthin microemulsion system, thereby fully exerting the efficacy of the astaxanthin and improving the shelf life stability of the astaxanthin.
The present invention will be described in detail with reference to examples.
Example 1
The preparation method of the astaxanthin eye cream comprises the following steps:
1) preparing free astaxanthin:
taking haematococcus pluvialis as a biological raw material for preparing esterified astaxanthin, weighing 1kg of haematococcus pluvialis powder, adding 10 times of absolute ethyl alcohol in the mass (W/V) of the raw material, repeatedly leaching for 2 times, leaching for 1 hour each time, combining leaching liquor, and then performing reduced pressure concentration on the leaching liquor to remove a solvent to obtain a crude extract; and then adding the crude extract into 30 times volume of 2% potassium hydroxide solution, performing saponification reaction at 4 ℃ under the condition of filling nitrogen, standing the reaction system at-2 ℃ for 2h after the reaction is finished, filtering, and collecting the crystallized and precipitated mauve substances to obtain the refined free astaxanthin.
2) Heat treatment of free astaxanthin:
weighing astaxanthin obtained in the step 1) according to a weight volume fraction (g/ml) of 2%, dissolving the astaxanthin in a dichloromethane solution, continuously carrying out heat treatment for 4 hours under the conditions of closed nitrogen charging and 70 ℃, and removing an organic solvent through reduced pressure concentration after the heat treatment to obtain the free astaxanthin after the heat treatment.
3) Preparing a free astaxanthin microemulsion:
adding the free astaxanthin after heat treatment into ethyl acetate according to the mass fraction of 1%, and stirring until the free astaxanthin is completely dissolved to form a free astaxanthin ethyl acetate solution; then sequentially adding 0.01 percent of vitamin E, 10 percent of Tween 80 and 5 percent of glycerol by mass volume fraction, and uniformly stirring; after stirring, evaporating and removing solvent residues under the conditions of low temperature and low pressure to prepare the free astaxanthin-rich nano microemulsion;
4) preparation of an aqueous phase: the aqueous solution was prepared to contain 0.2% by weight of xanthan gum, 10% by weight of absolute ethyl alcohol (containing 0.05% by weight of ethylparaben and 0.1% by weight of apple essence), and 0.01% by weight of tea polyphenols. The preparation method comprises the steps of dispersing all the components in deionized water, and fully stirring until all the components are dissolved to obtain a water phase.
5) Mixing and homogenizing: preheating the free astaxanthin nano microemulsion prepared in the step 3) and the aqueous phase solution of the step 4) to 60 ℃, and then adding the astaxanthin nano microemulsion into the aqueous phase according to the ratio of 1:1 while stirring. And (3) uniformly mixing, placing in a vacuum emulsifying machine, homogenizing and emulsifying for 15min, controlling the temperature to be 75 ℃ in the process, and then cooling to be 25 ℃ to obtain the astaxanthin eye cream capable of being efficiently absorbed.
Example 2
A preparation method of astaxanthin eye cream comprises the following steps:
1) preparing free astaxanthin: the method comprises the steps of taking haematococcus pluvialis as a biological raw material for preparing esterified astaxanthin, weighing 100g of haematococcus pluvialis powder, adding ethyl acetate with the mass (W/V) being 20 times that of the raw material, leaching for 4 hours, filtering, collecting leaching liquor, carrying out reduced pressure concentration on the leaching liquor, and removing a solvent to obtain a crude extract. Homogenizing and emulsifying Tween 80 with the mass of 1 time, adding phosphate buffer solution containing lipase at the dosage of 10U/μ g total astaxanthin, and performing enzymolysis at 40 deg.C and pH of 5.5 for 12 h. After enzymolysis, adding ethyl acetate into the system until demulsification is finished, collecting an oil phase, and performing reduced pressure concentration to obtain free astaxanthin;
2) heat treatment of free astaxanthin:
weighing astaxanthin obtained in the step 1), dissolving astaxanthin into ethyl acetate solution according to the weight volume fraction of 3%, and simultaneously adding powdery I-TiO with the weight volume fraction of 6%2Then continuously heat-treating for 2h under the conditions of closed nitrogen-filling and 60 ℃, filtering and recovering powdery I-TiO2And carrying out reduced pressure concentration on the solution to remove the organic solvent, thus obtaining the free astaxanthin after heat treatment.
3) Preparing free astaxanthin nano microemulsion: adding the free astaxanthin obtained in the step 2) after heat treatment into ethyl oleate according to the mass fraction of 0.5%, and stirring until the free astaxanthin is completely dissolved to form a free astaxanthin ethyl oleate solution; then adding coenzyme Q10 with the mass volume fraction of 0.01%, Tween 80 with the mass volume fraction of 10% and glycerol with the mass volume fraction of 5% in sequence, and uniformly stirring; after stirring, evaporating and removing solvent residues under the conditions of low temperature and low pressure to prepare the free astaxanthin-rich nano microemulsion;
4) preparation of an aqueous phase: the aqueous solution was prepared to contain 1% by weight of gelatin, 15% by weight of glycerin (containing 0.05% by weight of propylparaben and 0.1% by weight of mango essence), and 0.02% by weight of ascorbic acid. The preparation method comprises the steps of dispersing all the components in deionized water, and fully stirring until all the components are dissolved to obtain a water phase.
5) Mixing and homogenizing: preheating the free astaxanthin nano microemulsion prepared in the step 3) and the aqueous phase solution of the step 4) to 65 ℃, and then adding the astaxanthin nano microemulsion into the aqueous phase according to the ratio of 1:1.5 while stirring. Mixing, homogenizing and emulsifying in vacuum emulsifying machine for 20min at 70 deg.C, and cooling to 30 deg.C to obtain astaxanthin eye cream capable of being absorbed efficiently.
Example 3
A preparation method of astaxanthin eye cream comprises the following steps:
1) preparing free astaxanthin: weighing 100g of Phaffia rhodozyma, putting the Phaffia rhodozyma into an extraction kettle in a 1L supercritical extraction device, setting the temperature of the extraction kettle at 40 ℃, setting the pressure at 30MPa, and using an extractant CO2The flow rate of (A) was set to 20L/h, the temperature and pressure of the separation vessel I were 35 ℃ and 10MPa, respectively, the temperature of the separation vessel II was 40 ℃ and CO was set to2The flow rate of the fluid is 30L/h, the continuous dynamic extraction time is 3h, the extract is discharged from the separation kettle at irregular intervals, the extract is collected and stored in a container, and the extract is dark red viscous substance, so that crude extract rich in free astaxanthin is obtained; then refined free astaxanthin is obtained through column chromatography;
2) heat treatment of free astaxanthin: weighing astaxanthin obtained in the step 1), dissolving astaxanthin into dimethyl sulfoxide solution according to the weight volume fraction of 8%, and simultaneously adding powdery I-TiO with the weight volume fraction of 10%2Then continuously heat-treating for 2h under the conditions of closed nitrogen-filling and 70 ℃, filtering and recovering powdery I-TiO2Solutions ofAnd (4) carrying out reduced pressure concentration to obtain the free astaxanthin after heat treatment.
3) Preparing free astaxanthin nano microemulsion: adding free astaxanthin into olive oil according to the mass fraction of 0.1%, and stirring until the free astaxanthin is completely dissolved to form a free astaxanthin olive oil solution; then sequentially adding 0.01 percent of vitamin E, 8 percent of Tween 85 and 5 percent of ethanol by mass volume fraction, and uniformly stirring; after stirring, evaporating and removing solvent residues under the conditions of low temperature and low pressure to prepare the free astaxanthin-rich nano microemulsion;
4) preparation of an aqueous phase: the aqueous solution was prepared to contain 1% by weight of chitosan, 10% by weight of polyethylene glycol 400 (containing 0.05% by weight of propylparaben and 0.1% by weight of orange flavor), and 0.04% by weight of sodium edetate. The preparation method comprises the steps of dispersing all the components in deionized water, and fully stirring until all the components are dissolved to obtain a water phase.
5) Mixing and homogenizing: preheating the free astaxanthin nano microemulsion prepared in the step 3) and the aqueous phase solution of the step 4) to 70 ℃, and then adding the astaxanthin nano microemulsion into the aqueous phase according to the ratio of 1:2 while stirring. And (3) uniformly mixing, placing in a vacuum emulsifying machine, homogenizing and emulsifying for 10min, controlling the temperature to be 75 ℃ in the process, and then cooling to be 20 ℃ to obtain the astaxanthin eye cream capable of being efficiently absorbed.
Comparative example 4
A preparation method of astaxanthin eye cream comprises the following steps:
1) preparation of free astaxanthin: taking haematococcus pluvialis as a biological raw material for preparing esterified astaxanthin, weighing 1kg of haematococcus pluvialis powder, adding 10 times of absolute ethyl alcohol in the mass (W/V) of the raw material, repeatedly extracting for 2 times, extracting for 1 hour each time, combining extract liquor, then carrying out reduced pressure concentration on the extract liquor, removing a solvent, and obtaining a crude extract; and then adding the crude extract into 30 times volume of 2% potassium hydroxide solution, performing saponification reaction at 4 ℃ under the condition of filling nitrogen, standing the reaction system at-2 ℃ for 2h after the reaction is finished, filtering, and collecting the crystallized and precipitated mauve substances to obtain the refined free astaxanthin.
2) Preparing a free astaxanthin microemulsion: adding the free astaxanthin after heat treatment into ethyl acetate according to the mass fraction of 1%, and stirring until the free astaxanthin is completely dissolved to form a free astaxanthin ethyl acetate solution; then sequentially adding 0.01 percent of vitamin E, 10 percent of Tween 80 and 5 percent of glycerol by mass volume fraction, and uniformly stirring; after stirring, evaporating and removing solvent residues under the conditions of low temperature and low pressure to prepare the free astaxanthin-rich nano microemulsion;
3) preparation of an aqueous phase: the aqueous solution was prepared to contain 0.2% by weight of xanthan gum, 10% by weight of absolute ethyl alcohol (containing 0.05% by weight of ethylparaben and 0.1% by weight of apple essence), and 0.01% by weight of tea polyphenols. The preparation method comprises the steps of dispersing all the components in deionized water, and fully stirring until all the components are dissolved to obtain a water phase.
4) Mixing and homogenizing: preheating the free astaxanthin nano microemulsion prepared in the step 3) and the aqueous phase solution of the step 4) to 60 ℃, and then adding the astaxanthin nano microemulsion into the aqueous phase according to the ratio of 1:1 while stirring. And (3) uniformly mixing, placing in a vacuum emulsifying machine, homogenizing and emulsifying for 15min, controlling the temperature to be 75 ℃ in the process, and then cooling to be 25 ℃ to obtain the astaxanthin eye cream capable of being efficiently absorbed.
Example 5 detection: sunscreen and repair function testing
The test subjects were the astaxanthin eye cream sample prepared in example 1 and the eye cream sample of comparative example 4.
6 Kunming healthy mice with the mass of 20 +/-2 g are selected, and the male and female mice are divided into 2 groups randomly, and each group comprises 3 mice. Mice were prophylactically coated with test and control samples, 0.6mL per back, 0.3mL per single ear, 2/d, for a total of 4 d. The mouse is horizontally fixed on an iron stand and is irradiated for 6 hours at a vertical distance of 10cm from an ultraviolet lamp, so that a skin damage mouse model is formed. And (3) observing the change condition of the skin at the back of the mouse by taking the skin keratinization and desquamation degree of the mouse as evaluation indexes, and analyzing the protection effect of the sample on the skin of the mouse against ultraviolet injury.
Irradiating the skin damage mouse model with ultraviolet rays for 40h, cutting the spine, killing the mouse, weighing the mass of the mouse, then respectively taking two ears and a round ear piece and a round skin piece with the diameter of 9mm at the back, accurately weighing the mass of the mouse, calculating an ear index (ear index is ear piece mass/mouse mass) and a skin index (skin index is skin piece mass/mouse mass), and analyzing the inhibitory effect of the sample on the edema of the mouse injured by the ultraviolet rays. The skin on the back was fixed with 10% formaldehyde for 24 hours to prepare a mounting sample. Placing the sealed sample under a 10-time lens to observe the integral shape of the skin, then shooting a first picture from the uppermost end of the skin observed in a visual field under a 40-time lens, then shooting one picture every 2mm of a moving ruler, shooting 5 pictures, then selecting 5 points on each picture by using a microscopic image analysis system, measuring the thickness of the epidermis of the mouse, measuring 25 points in all pictures, taking an average value to record as the thickness of the epidermis, and analyzing the inhibition effect of the sample on the epidermal keratinization of the mouse. The number of fibroblasts in each field was counted and the mean value was recorded as the number of dermal fibroblasts in each field.
The results of the ultraviolet-damaged mouse ear index, skin index, epidermal thickness and fibroblast measurement are shown in Table 1.
Table 1: mouse ear index, skin index, epidermal thickness and fibroblast damaged by ultraviolet rays
The results showed that the ear index, skin index and thickness of the epidermis of the mice irradiated with ultraviolet rays were lower than those of the samples of the comparative examples, and the number of fibroblasts in the dermal tissue was larger than that of the control samples. Therefore, the test results show that the skin protection and repair effects of the astaxanthin eye cream can be remarkably improved by carrying out heat treatment on the free astaxanthin.
Example 6 stability testing
The astaxanthin eye cream samples prepared in example 1, example 2 and example 3 were stored at room temperature in the dark for 30 days, and the total astaxanthin retention rate was measured, and whether precipitation, delamination or an off-flavor was observed to evaluate the stability of the astaxanthin eye cream prepared according to the present invention, and the test results are shown in table 2.
The retention of total astaxanthin is calculated according to the following formula:
retention (%) of total astaxanthin ═ C30/C0×100％
Wherein, C0Is the total astaxanthin content in the starting sample; c30The astaxanthin content in the samples was determined after 30 days storage.
Table 2: results of stability test
As can be seen from the results in table 2, the astaxanthin stability in the astaxanthin eye cream prepared according to the present invention was good. Meanwhile, the prepared astaxanthin eye cream is stable in system, free of precipitation and stratification phenomena and free of peculiar smell.
Finally, it should be noted that the embodiments of the present invention are not limited to the above-mentioned embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.
Claims (5)
1. An astaxanthin eye cream is characterized in that the astaxanthin eye cream is prepared by using free astaxanthin after heat treatment as a raw material; wherein the heat-treated free astaxanthin is prepared by extracting astaxanthin from raw materials by solvent extraction method or supercritical fluid extraction method, treating the extracted astaxanthin by enzymolysis or saponification method, and heat-treating the treated product with solvent system to obtain heat-treated free astaxanthin;
the heat treatment of the solvent system is to add the astaxanthin treated by the enzymolysis or saponification method into the non-flammable low-boiling-point solvent and treat the astaxanthin for 0.5 to 50 hours at the temperature of 40 to 90 ℃; removing the organic solvent after the completion of the step to obtain the free astaxanthin after heat treatment; the non-flammable low-boiling point solvent is dichloromethane;
the preparation method of the astaxanthin eye cream comprises the following steps:
1) preparing free astaxanthin nano microemulsion:
adding free astaxanthin into carrier oil, and stirring to completely dissolve to form free astaxanthin oil solution; then adding an oil-soluble antioxidant, an emulsifier and/or an auxiliary emulsifier into the obtained oil solution, and uniformly stirring; removing solvent residues after stirring is finished, and preparing the free astaxanthin-rich nano microemulsion;
wherein the carrier oil is one or more of linear chain fatty acid ester and fatty glyceride;
the oil-soluble antioxidant is one or more of tocopherol, tocopherol acetate, coenzyme Q, gallate, butyl hydroxy anisole, dibutyl hydroxy toluene and carnosic acid;
the emulsifier is one or more of tween, span, poloxamer 188, polyoxyethylene castor oil, soybean phospholipid, lecithin, polyvinyl alcohol or polylactic acid-glycolic acid;
the auxiliary emulsifier is one or more of ethanol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol or polyethylene glycol;
2) preparation of an aqueous phase:
the water phase comprises the following components in percentage by weight: 0.1-2% of stabilizer, 0.5-15% of cosolvent, 0.001-3% of water-soluble antioxidant and the balance of deionized water;
the stabilizer is one or more of xanthan gum, lactalbumin, sodium caseinate, gelatin, polylysine, chitosan, albumin, acacia, sodium alginate and hydroxymethyl cellulose;
the cosolvent is one or more of ethanol, 1, 2-propylene glycol, 1, 3-propylene glycol, glycerol or polyethylene glycol,
the water-soluble antioxidant is one or more of tea polyphenol, ascorbic acid or sodium salt thereof, and ethylene diamine tetraacetic acid or sodium salt thereof;
3) mixing and homogenizing: preheating the free astaxanthin nano microemulsion prepared in the step 1) and the aqueous phase solution prepared in the step 2) to 40-80 ℃, and then adding the astaxanthin nano microemulsion into the aqueous phase according to the proportion of 1: 0.3-4 while stirring; after being uniformly mixed, the mixture is put into a vacuum emulsifying machine for homogenizing and emulsifying for 5-30 min, the temperature is controlled to be 40-80 ℃ in the process, and then the temperature is reduced to 10-35 ℃ to finish the preparation.
2. The astaxanthin eye cream of claim 1, wherein powdered I-TiO is further added during the heat treatment2As a catalyst for the heat treatment process.
3. The astaxanthin eye cream according to claim 1, wherein the solvent is one or more of absolute ethyl alcohol, acetone, ethyl acetate, methylene chloride and n-hexane.
4. The astaxanthin eye cream of claim 1, wherein the raw material is Haematococcus pluvialis or Phaffia rhodozyma.
5. The astaxanthin eye cream as claimed in claim 1, wherein the aqueous phase of step 2) further comprises a preservative and a fruit essence.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910592257.3A CN110179684B (en) | 2019-07-01 | 2019-07-01 | Natural astaxanthin eye cream capable of being efficiently absorbed and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910592257.3A CN110179684B (en) | 2019-07-01 | 2019-07-01 | Natural astaxanthin eye cream capable of being efficiently absorbed and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110179684A CN110179684A (en) | 2019-08-30 |
| CN110179684B true CN110179684B (en) | 2022-05-10 |
Family
ID=67724723
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910592257.3A Active CN110179684B (en) | 2019-07-01 | 2019-07-01 | Natural astaxanthin eye cream capable of being efficiently absorbed and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110179684B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110448482B (en) * | 2019-09-27 | 2020-06-09 | 瑞希(重庆)生物科技有限公司 | Emulsion and preparation method thereof |
| CN113842332B (en) * | 2021-09-02 | 2024-01-26 | 青岛优度生物工程有限公司 | Lip glaze and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20110130036A (en) * | 2010-05-27 | 2011-12-05 | (주)뉴트리 | Nanoemulsion composition comprising astaxanthin |
| WO2013002479A2 (en) * | 2011-06-28 | 2013-01-03 | 한국콜마 주식회사 | Nanoemulsion composition and method for preparing same |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104042568B (en) * | 2014-06-23 | 2016-06-29 | 青岛优度生物工程有限公司 | A kind of astaxanthin nano-emulsion preparation and preparation method thereof |
| CN104352434B (en) * | 2014-11-20 | 2018-05-18 | 中国海洋大学 | A kind of high stability astaxanthin ester is from microemulsion and preparation method thereof |
| CN105087738A (en) * | 2015-09-12 | 2015-11-25 | 中国海洋大学 | Method for preparing natural astaxanthin through microemulsion phase biotransformation |
| CN106580762B (en) * | 2016-12-22 | 2019-10-18 | 广州睿森生物科技有限公司 | Have effects that comfort the crease-resistant composite skin care product of line, eye cream and preparation method thereof |
| CN107307403B (en) * | 2017-07-12 | 2021-01-01 | 日照职业技术学院 | Astaxanthin micro-nano solid preparation |
| CN108516947A (en) * | 2018-04-27 | 2018-09-11 | 云南省药物研究所 | A kind of refined natural astaxanthin（Oil）Method |
| CN109303220A (en) * | 2018-11-14 | 2019-02-05 | 日照职业技术学院 | A kind of astaxanthin functional sport drink and preparation method thereof |
-
2019
- 2019-07-01 CN CN201910592257.3A patent/CN110179684B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20110130036A (en) * | 2010-05-27 | 2011-12-05 | (주)뉴트리 | Nanoemulsion composition comprising astaxanthin |
| WO2013002479A2 (en) * | 2011-06-28 | 2013-01-03 | 한국콜마 주식회사 | Nanoemulsion composition and method for preparing same |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110179684A (en) | 2019-08-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110179685B (en) | Essence containing natural astaxanthin | |
| JP2008044939A (en) | Slimming composition for cosmetic containing extract of biomass of alga neochloris oleoabundans | |
| CN110179684B (en) | Natural astaxanthin eye cream capable of being efficiently absorbed and preparation method thereof | |
| CN115887518A (en) | Anti-glycation application of sweet wormwood herb extract | |
| KR102065607B1 (en) | cosmetic composition for skin moisturizing and skin elasticity using palm oil fraction | |
| WO2011019875A2 (en) | Antioxidant dietary supplement compositions | |
| CN109512734B (en) | External plant extract and cosmetic with skin elasticity and gloss recovery effects and preparation method thereof | |
| CA2723835C (en) | Echinoderm-derived extracts, methods of preparation and uses thereof | |
| CN102105142B (en) | Compositions for treating rosacea comprising chitosan and a dicarboxylic acid | |
| KR100955572B1 (en) | Cosmetic composition comprising a supercritical fluid extract of Morinda citrifolia | |
| JP5770426B2 (en) | Singlet oxygen scavenger, skin external preparation and cosmetic using the singlet oxygen scavenger | |
| KR20180027772A (en) | Cosmetic composition for preventing near infrared ray containing extract of ganoderma lucidum | |
| JP2009143849A (en) | Anti-aging agent, skin whitening agent, antioxidant, anti-inflammatory agent, and humectant | |
| JP2009209063A (en) | Skin preparation for external use, or skin cosmetic | |
| CN109689026A (en) | Increase the method for lipolysis using the composition comprising bioactivity lotus (NELUMBO NUCIFERA) extract | |
| KR101577118B1 (en) | Cosmetic Composition for Moisturizing Containing Red Ginseng Butter as an Active Ingredient | |
| WO2015049265A1 (en) | Oily composition containing an extract of daylily and uses thereof | |
| JP4748962B2 (en) | Moisturizer, cell activator, whitening agent, and antioxidant | |
| CN114366685B (en) | Preparation method and application of red clover isoflavone phytosterol liposome | |
| KR100570095B1 (en) | Cosmetic Composition for Improving Skin Wrinkle Containing Supercritical Extract of Glycine max Merr as Active Ingredient | |
| JP4994684B2 (en) | Moisturizer, cell activator, and antioxidant | |
| JP2004137166A (en) | Skin care preparation for external use, cell activator and antioxidant | |
| CN109512733B (en) | External plant extract and cosmetic with effects of nourishing and moistening hand skin and preparation method thereof | |
| KR100604091B1 (en) | Cosmetic Composition for Abirritating Skin Containing Extract of Black Soybean as Active Ingredient | |
| Peranginangin et al. | Antioxidant Activity Test of the Red Yeast Rice Extract and the Formulation in a Cream Preparations Andit’S Penetration and Safety Test At Rabbit |
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 |