CN115531224B - Whitening anti-aging skin brightening liquid and preparation method thereof - Google Patents
Whitening anti-aging skin brightening liquid and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of cosmetics, and discloses a whitening and anti-aging skin-brightening liquid and a preparation method thereof, wherein the whitening and anti-aging skin-brightening liquid comprises the following raw materials in parts by weight: 30-40 parts of cationic cyclodextrin, 1-2 parts of phenethyl resorcinol, 3-5 parts of honeysuckle flavone complex, 0.5-2 parts of citrus peel extract, 0.5-1 part of daisy flower extract, 0.1-0.5 part of pulsatilla root extract, 1-3 parts of glycerol and 80-150 parts of deionized water, and the phenethyl resorcinol and honeysuckle flavone complex which are not easy to be compatible are included by using the cationic cyclodextrin and are combined with the citrus peel extract and the daisy flower extract, so that deep whitening anti-aging ways from the surface to the inside are mutually cooperated, and the whitening effect of the whitening anti-aging skin-brightening liquid is exerted.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to a whitening anti-aging skin brightening liquid and a preparation method thereof.
Background
With the increase of age, the human body is affected by various factors, progressive morphological structure and physiological function decline can be generated, wherein skin is taken as the largest organ of the human body, the aging process is also inevitably managed, skin problems such as wrinkles, slacks, spots and the like are gradually increased along with the aging of the skin, the skin problems easily cause anxiety and the like, even influence the mental state of people, in recent years, the beauty technology of mainly beating whitening anti-aging flag is developed rapidly, and skin brightening liquid and other cosmetics mainly playing the role of whitening anti-aging are layered, but most of whitening anti-aging cosmetics do not have fine research on raw materials, and the synergy and complementation of the drug effect among all the components are not fully explored, so that a cosmetic with mutual synergy among the components and remarkable whitening anti-aging effect is developed, and the cosmetic has great significance.
The phenethyl resorcinol is a high-activity tyrosinase inhibitor, and because tyrosinase is a key speed-limiting enzyme in the melanin synthesis process, the phenethyl resorcinol can reduce the melanin synthesis speed and quantity by inhibiting the activity of the tyrosinase inhibitor, and meanwhile, the phenethyl resorcinol also has good antioxidant and antibacterial capabilities, so that the phenethyl resorcinol can play a good skin whitening effect when being applied to whitening anti-aging cosmetics, but the phenethyl resorcinol has poor solubility, is difficult to be compatible with other components, is unstable, is easy to oxidize and change color, is difficult to enter a whitening target part through a skin cuticle, and has certain skin irritation, so that the phenethyl resorcinol is difficult to be practically applied to the whitening anti-aging cosmetics.
The honeysuckle flavonoid compound can absorb ultraviolet rays, promote skin cell growth, help skin discharge toxin, enable skin to be smooth and white, and simultaneously can resist bacteria, diminish inflammation and eliminate free radicals, so that the honeysuckle flavonoid compound is very suitable for research and development of whitening anti-aging cosmetics, but the honeysuckle flavonoid compound has limited free radical scavenging efficiency, is difficult to exert strong oxidation resistance, further achieves the anti-aging purpose, and has poor solubility, is difficult to form good compatibility with other components in cosmetics, and further needs to be compounded with other substances to enhance the free radical scavenging capability, so that the honeysuckle flavonoid compound has better anti-aging performance.
The citrus peel extract has excellent antibacterial and anti-inflammatory properties, has certain anticancer, beautifying and nourishing effects, can be applied to medicines, can be applied to the field of cosmetics, contains rich functional components such as tannin, saponin, mucus and the like, can repair the fragile skin after sun-drying, arouse the dull and tired skin, and can also astringe the skin to enable the skin to be smoother, so that the citrus peel extract has a plurality of applications in the field of cosmetics.
Disclosure of Invention
The invention aims to provide a whitening anti-aging skin brightening liquid and a preparation method thereof, which solve the following technical problems:
(1) Solves the problems that the solubility of phenethyl resorcinol and honeysuckle flavonoid compounds is poor and the phenethyl resorcinol and honeysuckle flavonoid compounds are difficult to be compatible with other components in skin brightening liquid.
(2) Solves the problems of low free radical removal rate and poor oxidation resistance of a single honeysuckle flavonoid compound, resulting in poor anti-aging performance of the skin brightening liquid.
(3) Reduces the skin irritation of phenethyl resorcinol and widens the application range of skin brightening liquid.
The aim of the invention can be achieved by the following technical scheme:
the whitening anti-aging skin brightening liquid consists of the following components in parts by weight: 30-40 parts of cationic cyclodextrin, 1-2 parts of phenethyl resorcinol, 3-5 parts of honeysuckle flavone complex, 0.5-2 parts of citrus peel extract, 0.5-1 part of daisy flower extract, 0.1-0.5 part of pulsatilla root extract, 1-3 parts of glycerol and 80-150 parts of deionized water;
the cationic cyclodextrin is prepared by chemical reaction of 2-hydroxypropyl-beta-cyclodextrin and 3-chloro-2-hydroxypropyl trimethyl ammonium chloride;
the honeysuckle flavone complex is prepared by taking a honeysuckle flavone extract and metal salt as raw materials and carrying out meridian-collateral reaction.
Further, the chemical reaction specifically includes: dissolving 2-hydroxypropyl-beta-cyclodextrin in deionized water, adding sodium hydroxide solution, fully and uniformly mixing, continuously adding 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, heating to 70-90 ℃, stirring for reaction for 2-8h, regulating the pH value of the reaction solution to be neutral by using hydrochloric acid solution after the reaction is finished, carrying out suction filtration on the reaction solution, collecting filter residues, washing the filter residues for 2-4 times, and carrying out vacuum drying to obtain the cationic cyclodextrin.
Further, the mass concentration of the sodium hydroxide solution is 20-40%.
Further, the mass concentration of the hydrochloric acid solution is 10-15%.
Through the technical scheme, in the alkaline environment provided by the sodium hydroxide solution, the hydroxyl in the 2-hydroxypropyl-beta-cyclodextrin structure can react with the chlorine-containing group in the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride structure in a nucleophilic substitution manner, so that abundant quaternary ammonium salt functional groups are introduced into the 2-hydroxypropyl-beta-cyclodextrin structure, and the charge attribute of cyclodextrin is changed, and the cyclodextrin derivative containing cations is obtained.
Further, the complexation specifically includes the following steps:
s1: pulverizing flos Lonicerae, and sieving with 20-40 mesh sieve to obtain flos Lonicerae powder;
s2: adding flos Lonicerae powder into 60-80% ethanol solution at a liquid-material ratio of 1:10-30, placing into an ultrasonic instrument, setting ultrasonic power to 200-300W, extracting at 40-60deg.C for 30-60min for 2-4 times, filtering to obtain residue, mixing extractive solutions, and freeze drying to obtain flos Lonicerae flavone extract;
s3: adding the honeysuckle flavone extract into absolute ethyl alcohol, fully stirring and dissolving, regulating the pH of the solution by using triethylamine, adding metal salt, stirring and mixing, heating to 50-60 ℃, stirring and reacting for 4-12 hours, after the reaction liquid is completely cooled, filtering, separating out a solid product, washing for 2-4 times by using a mixed solution of ethyl alcohol and deionized water, and vacuum drying to obtain the honeysuckle flavone complex.
Further, in step S3, the pH is adjusted to 8-9.
Further, in step S3, the metal salt is any one of ferric chloride and cupric chloride.
Further, in step S3, the volume ratio of the ethanol to the deionized water is 1:1.
According to the technical scheme, honeysuckle flower flavone is extracted by crushing and sieving honeysuckle flower, so that the granularity of the honeysuckle flower flavone is reduced, extraction of active ingredients of the honeysuckle flower flavone is facilitated, and the honeysuckle flower flavone is complexed with copper ions or iron ions to obtain a honeysuckle flower flavone complex, so that the honeysuckle flower flavone has stronger oxidation resistance.
The preparation method of the whitening anti-aging skin brightening liquid specifically comprises the following steps:
SS1: mixing phenethyl resorcinol and a honeysuckle flavone complex, and dissolving the mixture in an ethanol solvent according to a liquid-to-material ratio of 1:5-10 to obtain a premix;
SS2: adding cationic cyclodextrin into deionized water according to a liquid-to-material ratio of 1:10-20, fully stirring to form cationic cyclodextrin aqueous solution, pouring the premixed solution prepared in the step SS1 into the aqueous solution, uniformly mixing, transferring the system into a water bath oscillator, oscillating at a rotating speed of 80-100rpm for 8-12h at a temperature of 20-40 ℃, filtering out precipitate in the solution by using a microporous filter membrane, carrying out vacuum drying, and grinding and crushing the dried product to obtain a cationic cyclodextrin inclusion compound;
SS3: adding deionized water, cationic cyclodextrin clathrate, citrus peel extract, daisy flower extract, radix Pulsatillae extract and glycerol into a high-speed stirrer, stirring uniformly at a rotation speed of 200-500r/min, discharging, and packaging after inspection is qualified to obtain the whitening and anti-aging skin brightening liquid.
Further, in step SS2, the pore size of the microporous filter membrane is 0.5-3um.
According to the technical scheme, phenethyl resorcinol and honeysuckle flavone complex are used as objects, cationic cyclodextrin is used for clathrating the objects to form cationic cyclodextrin inclusion compound, pulsatilla chinensis extract is used as a plant preservative, and glycerin is used as a humectant, and due to the fact that cyclodextrin has a special amphiphilic structure with inner hydrophobic property and outer hydrophilic property, the solubility of the phenethyl resorcinol and honeysuckle flavone complex can be improved, the phenethyl resorcinol and honeysuckle flavone complex is easier to be compatible with components such as citrus peel extract, daisy flower extract, pulsatilla chinensis extract and glycerin, and the cyclodextrin can be combined with lipid on skin in a reversible way, a certain hydration effect can be achieved on skin, and the permeability of skin is improved, so that the percutaneous permeation rate of the phenethyl resorcinol and honeysuckle flavone complex is improved.
The invention has the beneficial effects that:
(1) According to the invention, phenethyl resorcinol, honeysuckle flavone complex, citrus peel extract and daisy extract are used as main components of the whitening anti-aging skin brightening liquid, and can be used for blocking the formation of skin melanin at different stages, wherein the honeysuckle flavone complex can absorb ultraviolet rays, reduce the ageing and pigmentation phenomena of the skin caused by sunlight irradiation, phenethyl resorcinol can inhibit tyrosinase activity, reduce the synthesis speed and quantity of melanin, the citrus peel extract can promote the transfer of melanin to keratinocytes and gradually become epidermis or other substances, finally, the cornified fall-off is realized, the daisy extract can improve the activity of melanocyte, promote melanocyte phagocytosis, and discharge the melanin from the body through a circulatory system, so that deep-level whitening ways from the surface to the inside are formed to cooperate with each other, and the whitening effect of the anti-aging skin brightening liquid is exerted.
(2) According to the invention, the honeysuckle flavone complex is adopted as a component playing an anti-aging role in the whitening anti-aging skin brightening liquid, and the complex is formed by using iron or copper ions and the honeysuckle flavone, so that the honeysuckle flavone is easier to provide electrons to combine with free radicals by virtue of coordination between the honeysuckle flavone and central metal ions, and a more stable semi-quinone free radical structure is formed, so that stronger oxidation resistance can be displayed, and therefore, compared with the honeysuckle flavone compound, the honeysuckle flavone complex has stronger free radical scavenging capability and better oxidation aging resistance.
(3) According to the invention, the cationic cyclodextrin is adopted to carry out inclusion on the phenethyl resorcinol and the honeysuckle flavone complex, and because the sebum and the cell surface of the human body are electronegative, the cationic cyclodextrin inclusion compound can be adsorbed on the sebum surface through electrostatic interaction and gradually penetrate through the stratum corneum to enter the deep layer of the skin to be combined with the cell, so that the phenethyl resorcinol and the honeysuckle flavone complex are released, the combination of the phenethyl resorcinol and the honeysuckle flavone complex with whitening anti-aging targets is promoted, the maximum efficacy of the phenethyl resorcinol and the honeysuckle flavone complex is exerted, and thus the whitening anti-aging effect is realized.
Of course, it is not necessary for any one product to practice the invention to achieve all of the advantages set forth above at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a Zeta potential diagram of 2-hydroxypropyl-beta-cyclodextrin;
FIG. 2 is a Zeta potential diagram of cationic cyclodextrin prepared in example 1 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
1. Preparation of cationic cyclodextrins
Dissolving 2g of 2-hydroxypropyl-beta-cyclodextrin in deionized water, adding a sodium hydroxide solution with the mass concentration of 30%, fully and uniformly mixing, continuously adding 1.2g of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, heating to 85 ℃, stirring and reacting for 4 hours, adjusting the pH of a reaction solution to be neutral by using a hydrochloric acid solution with the mass concentration of 10% after the reaction is finished, carrying out suction filtration on the reaction solution, collecting filter residues, washing the filter residues for 3 times, carrying out vacuum drying to obtain cationic cyclodextrin, preparing 10g/L of saturated solution of 2-hydroxypropyl-beta-cyclodextrin and cationic cyclodextrin, analyzing the saturated solution by using an HL8001 type Zeta potential analyzer, wherein the analysis result is shown in figures 1 and 2, the Zeta potential of the 2-hydroxypropyl-beta-cyclodextrin is about 20mV, the Zeta potential of the 2-hydroxypropyl-beta-cyclodextrin is presumed to be negative in the water solution, the Zeta potential of the cationic cyclodextrin is about 10mV, and the Zeta potential of the cationic cyclodextrin is presumed to be higher than the Zeta potential of the cationic cyclodextrin in the cationic cyclodextrin structure of the 2-hydroxypropyl-beta-cyclodextrin.
2. Preparation of honeysuckle flavone complex
S1: pulverizing flos Lonicerae, and sieving with 20 mesh sieve to obtain flos Lonicerae powder;
s2: adding flos Lonicerae powder into 70% ethanol solution at a liquid-to-material ratio of 1:15, placing into an ultrasonic instrument, setting ultrasonic power to 250W, extracting at 50deg.C for 40min for 3 times, filtering to obtain residue, mixing extractive solutions, and freeze drying to obtain flos Lonicerae flavone extract;
s3: adding the honeysuckle flavone extract into absolute ethyl alcohol, fully stirring and dissolving, regulating the pH value of the solution to 8 by using triethylamine, adding copper chloride, stirring and mixing, heating to 60 ℃, stirring and reacting for 8 hours, after the reaction liquid is completely cooled, carrying out suction filtration, separating out solid products, washing 3 times by using the mixed solution of ethyl alcohol and deionized water with the volume ratio of 1:1, carrying out vacuum drying to obtain a honeysuckle flavone complex, weighing 2mg of the honeysuckle flavone extract and the honeysuckle flavone complex, measuring the percentage content of organic elements C, H by using a TQ-3A type element analyzer, respectively weighing 5mg of the honeysuckle flavone extract and the honeysuckle flavone complex, calcining for 3 hours at 500 ℃ in a muffle furnace, weighing, estimating the mass fraction of copper elements in the complex, and testing the results shown in the table below:
TABLE 1 elemental content analysis
As can be seen from the above table, compared with the honeysuckle flavone extract, the percentage content of C and H elements of the honeysuckle flavone complex is reduced, the percentage content of copper element is greatly increased, and it is presumed that the copper chloride and the honeysuckle flavone extract undergo a complexation reaction to form the honeysuckle flavone complex.
3. Preparation of whitening anti-aging skin brightening liquid
SS1: 1 part of phenethyl resorcinol and 3 parts of honeysuckle flavone complex are mixed and dissolved in an ethanol solvent according to a liquid-to-material ratio of 1:5 to obtain a premix;
SS2: adding 30 parts of cationic cyclodextrin into deionized water according to a liquid-to-material ratio of 1:10, fully stirring uniformly to form cationic cyclodextrin aqueous solution, pouring the premixed solution prepared in the step SS1 into the aqueous solution, uniformly mixing, transferring the system into a water bath oscillator, oscillating for 8 hours at a speed of 80rpm at a temperature of 20 ℃, filtering out precipitate in the solution by using a microporous filter membrane with a pore diameter of 0.5um, vacuum drying, and grinding and crushing the dried product to obtain a cationic cyclodextrin inclusion compound;
SS3: adding 80 parts of deionized water, cationic cyclodextrin inclusion compound, 0.5 part of citrus peel extract, 0.5 part of daisy flower extract, 0.1 part of pulsatilla root extract and 1 part of glycerol into a high-speed stirrer, starting stirring, uniformly stirring at a rotating speed of 200r/min, discharging, and filling after the inspection is qualified to obtain the whitening anti-aging skin brightening liquid.
Example 2
Preparation of whitening anti-aging skin brightening liquid
SS1: mixing 1.5 parts of phenethyl resorcinol and 4 parts of honeysuckle flavone complex, and dissolving in an ethanol solvent according to a liquid-to-material ratio of 1:8 to obtain a premix;
SS2: adding 35 parts of cationic cyclodextrin into deionized water according to a liquid-to-material ratio of 1:15, fully stirring uniformly to form cationic cyclodextrin aqueous solution, pouring the premixed solution prepared in the step SS1 into the aqueous solution, uniformly mixing, transferring the system into a water bath oscillator, oscillating for 9 hours at a temperature of 30 ℃ at a rotating speed of 80rpm, filtering out precipitate in the solution by using a microporous filter membrane with a pore diameter of 2um, drying in vacuum, and grinding and crushing the dried product to obtain a cationic cyclodextrin inclusion compound;
SS3: 120 parts of deionized water, cationic cyclodextrin inclusion compound, 1.5 parts of citrus peel extract, 0.8 part of daisy flower extract, 0.4 part of pulsatilla root extract and 2 parts of glycerin are added into a high-speed stirrer, stirring is started, stirring is uniform at the rotating speed of 400r/min, discharging is carried out, and filling is carried out after inspection is qualified, so that the whitening anti-aging skin brightening liquid is obtained.
The preparation method of the cationic cyclodextrin and honeysuckle flavone complex is the same as that of the example 1.
Example 3
Preparation of whitening anti-aging skin brightening liquid
SS1: 2 parts of phenethyl resorcinol and 5 parts of honeysuckle flavone complex are mixed and dissolved in an ethanol solvent according to a liquid-to-material ratio of 1:10 to obtain a premix;
SS2: adding 40 parts of cationic cyclodextrin into deionized water according to a liquid-to-material ratio of 1:20, fully stirring uniformly to form cationic cyclodextrin aqueous solution, pouring the premixed solution prepared in the step SS1 into the aqueous solution, uniformly mixing, transferring the system into a water bath oscillator, oscillating for 12 hours at a temperature of 40 ℃ at a rotating speed of 100rpm, filtering out precipitate in the solution by using a microporous filter membrane with a pore diameter of 3um, drying in vacuum, and grinding and crushing the dried product to obtain a cationic cyclodextrin inclusion compound;
SS3: 150 parts of deionized water, cationic cyclodextrin inclusion compound, 2 parts of citrus peel extract, 1 part of daisy flower extract, 0.5 part of pulsatilla chinensis extract and 3 parts of glycerol are added into a high-speed stirrer, stirring is started, stirring is uniform at the rotating speed of 500r/min, discharging is carried out, and filling is carried out after inspection is qualified, so that the whitening anti-aging skin brightening liquid is obtained.
The preparation method of the cationic cyclodextrin and honeysuckle flavone complex is the same as that of the example 1.
Comparative example 1
Preparation of whitening anti-aging skin brightening liquid
SS1: mixing 1.5 parts of phenethyl resorcinol and 4 parts of honeysuckle flavone extract, and dissolving in an ethanol solvent according to a liquid-to-material ratio of 1:8 to obtain a premix;
SS2: adding 35 parts of cationic cyclodextrin into deionized water according to a liquid-to-material ratio of 1:15, fully stirring uniformly to form cationic cyclodextrin aqueous solution, pouring the premixed solution prepared in the step SS1 into the aqueous solution, uniformly mixing, transferring the system into a water bath oscillator, oscillating for 9 hours at a temperature of 30 ℃ at a rotating speed of 80rpm, filtering out precipitate in the solution by using a microporous filter membrane with a pore diameter of 2um, drying in vacuum, and grinding and crushing the dried product to obtain a cationic cyclodextrin inclusion compound;
SS3: 120 parts of deionized water, cationic cyclodextrin inclusion compound, 1.5 parts of citrus peel extract, 0.8 part of daisy flower extract, 0.4 part of pulsatilla root extract and 2 parts of glycerin are added into a high-speed stirrer, stirring is started, stirring is uniform at the rotating speed of 400r/min, discharging is carried out, and filling is carried out after inspection is qualified, so that the whitening anti-aging skin brightening liquid is obtained.
The preparation method of the cationic cyclodextrin and the honeysuckle flavone extract is the same as that of the example 1.
Comparative example 2
Preparation of whitening anti-aging skin brightening liquid
SS1: mixing 1.5 parts of phenethyl resorcinol and 4 parts of honeysuckle flavone complex, and dissolving in an ethanol solvent according to a liquid-to-material ratio of 1:8 to obtain a premix;
SS2: adding 35 parts of 2-hydroxypropyl-beta-cyclodextrin into deionized water according to a liquid-to-material ratio of 1:15, fully stirring to form a cyclodextrin aqueous solution, pouring the premixed solution prepared in the step SS1 into the aqueous solution, uniformly mixing, transferring the system into a water bath oscillator, oscillating for 9 hours at a temperature of 30 ℃ at a rotating speed of 80rpm, filtering out a precipitate in the solution by using a microporous filter membrane with a pore diameter of 2um, carrying out vacuum drying, and carrying out grinding and crushing on the dried product to obtain a cyclodextrin inclusion compound;
SS3: 120 parts of deionized water, cyclodextrin inclusion compound, 1.5 parts of citrus peel extract, 0.8 part of daisy flower extract, 0.4 part of pulsatilla root extract and 2 parts of glycerin are added into a high-speed stirrer, stirring is started, stirring is uniform at the rotating speed of 400r/min, discharging is carried out, and filling is carried out after inspection is qualified, so that the whitening anti-aging skin brightening liquid is obtained.
The preparation method of the honeysuckle flavone complex is the same as that of the example 1.
Performance test of whitening anti-aging skin-brightening liquid prepared in example 1-example 3 and comparative example 1-comparative example 2 of the present invention:
(1) experiment of irritation
Referring to skin irritation/corrosiveness experiments in cosmetic health Specification, 50 healthy rabbits weighing 180-220g were selected and divided into five groups of 10 rabbits each, the back hair of each group was scraped out of a 2cm×2cm area, a whitening anti-aging skin brightening liquid was applied to the place, and the skin phenomenon at the place was recorded, and the results are shown in the following table:
TABLE 2 skin irritation response criteria
TABLE 3 skin irritation test results
As can be seen from the table, the whitening anti-aging skin brightening liquid prepared by the invention is warm and has no stimulation, and is applicable to a wide range of people.
(2) Experiments on whitening effect
The sterile conditions were strictly controlled and the mouse melanoma cells B16F10 were inoculated in culture flasks containing 10% (v/v) fetal bovine serum DMEM medium at 37℃with 5% CO 2 Is digested and passaged every 2 days by trypsin with a mass concentration of 0.25%, the cultured second generation melanoma cells are inoculated into a 12-well plate at a density of 104 times/mL, the liquid is changed after 24 hours, and 2mL of the whitening and anti-aging skin brightening liquid prepared in example 1-example 3 and comparative example 1-comparative example 2 are added, 3 wells are added to each group of samples, and the temperature is 37 ℃ and the concentration of CO is 5% 2 Removing supernatant, washing with 1mL of PBS buffer in each air for 2 times, adding 500uL of trypsin, digesting at 37deg.C for 5 min, adding 1mL of PBS buffer after 5 min to terminate digestion, centrifuging for 4min, collecting cells, discarding supernatant, and adding into each well200uL of polyethylene glycol octyl phenyl ether with the mass concentration of 0.1% is added, after uniform mixing, the mixture is frozen for 30min at the temperature of minus 20 ℃, taken out, cracked for half an hour at the temperature of 4 ℃, centrifuged for 10min after cracking, the supernatant is discarded, 100uL of dimethyl sulfoxide solution containing 1% sodium hydroxide is added into each group of samples, the mixture is treated for 2h at the temperature of 90 ℃, the supernatant is taken after centrifugation for 10min, a 96-well plate is added, the optical density result is read by an enzyme-labeling instrument at the wavelength of 490nm, the melanin content of cells treated by the blank is taken as a reference, the reduction amount of the melanin content in the cells is calculated, and the test result is shown in table 4:
TABLE 4 whitening effect test results
Note that: mouse melanoma cells B16F10 were purchased from wushang biosciences ltd.
The experiment selects the mouse melanoma cell B16F10 which can generate melanin under normal conditions, and the function of the melanoma cell for synthesizing the melanin is basically consistent with that of normal human melanocytes, so that the whitening effect of the whitening anti-aging skin brightening liquid can be reflected through the reduction degree of the melanin content in the mouse melanoma cell B16F 10. As can be seen from the data in table 4, the whitening anti-aging skin-brightening liquid prepared in examples 1 to 3 and comparative example 1 of the present invention has a strong whitening effect, presumably because the cationic cyclodextrin is used to clathrate the whitening component, so that the whitening component is easier to enter the cells, and further a better whitening effect is exerted, and the conventional cyclodextrin used in comparative example 2 is used to clathrate the whitening component, so that the whitening component cannot be promoted to enter the cells through electrostatic adsorption, resulting in a slightly poorer whitening effect.
(3) Anti-aging test
Taking 60 mice with the weight of 20-25g, dividing the mice into 6 groups, continuously filling the mice with 1.2mL/kg of the liquid into the stomach for 3 weeks, one time a day, after the last time of filling the stomach, fasted all the mice, killing the mice after the empty stomach is kept for 24 hours, taking the blood of the mice, adding 80uL of heparin sodium into the blood, preventing coagulation, centrifuging for 10 minutes at the rotating speed of 3500r/min, taking the supernatant blood, pouring the serum into a test tube according to the instruction of a malondialdehyde test box, sequentially adding reagents and application liquid, fully mixing, taking out after reacting for 40 minutes at 95 ℃, centrifuging for 10 minutes at the rotating speed of 3500r/min after cooling, taking the supernatant, measuring the absorbance value in the test tube at 532nm, calculating the Malondialdehyde (MDA) content in the serum, taking a blank tube as a control group, simultaneously taking another part of serum, pouring the serum into a test tube according to the instruction of a superoxide dismutase (SOD) test box, sequentially adding the reagents and the application liquid, mixing, standing at the room temperature for 10 minutes, and measuring the absorbance value in the test tube at 550nm, and testing the same time, and testing the test tube and the same table and comparing the absorbance value in the test tube.
TABLE 5 anti-aging test results
Note that: ★ representing significant differences between groups, P < 0.05, malondialdehyde test box and superoxide dismutase test box were purchased from Shanghai Hengyuan Biotech Co.
Oxygen free radicals are generated in organisms and can attack unsaturated fatty acid in biological membranes so as to cause lipid peroxides such as malondialdehyde and the like to form, the lipid peroxides can cause cell metabolism and dysfunction, and superoxide dismutase plays a role in eliminating superoxide free radicals in the organisms and preventing cells from being damaged, so that the content of malondialdehyde and superoxide dismutase can be measured to react with the aging degree of cells in the organisms, and as can be seen from the data in Table 5, the whitening and antioxidant skin brightening liquid prepared in the embodiment 1-embodiment 3 of the invention has good anti-aging performance, the whitening and antioxidant skin brightening liquid prepared in the comparative example 1 has general anti-aging performance due to the added honeysuckle flavone extract, and the whitening and antioxidant skin brightening liquid prepared in the comparative example 2 cannot absorb cosmetic components on sebum through electrostatic interaction due to the fact that cationic cyclodextrin is not used, and further the honeysuckle flavone complex penetrates through stratum corneum and enters the deep skin, so that the anti-aging performance is also general.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (8)
1. The whitening anti-aging skin brightening liquid is characterized by comprising the following components in parts by weight: 30-40 parts of cationic cyclodextrin, 1-2 parts of phenethyl resorcinol, 3-5 parts of honeysuckle flavone complex, 0.5-2 parts of citrus peel extract, 0.5-1 part of daisy flower extract, 0.1-0.5 part of pulsatilla root extract, 1-3 parts of glycerol and 80-150 parts of deionized water;
the cationic cyclodextrin is prepared by chemical reaction of 2-hydroxypropyl-beta-cyclodextrin and 3-chloro-2-hydroxypropyl trimethyl ammonium chloride;
the chemical reaction specifically comprises the following steps: dissolving 2-hydroxypropyl-beta-cyclodextrin in deionized water, adding sodium hydroxide solution, fully and uniformly mixing, continuously adding 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, heating to 70-90 ℃, stirring for reacting for 2-8 hours, regulating the pH value of the reaction solution to be neutral by using hydrochloric acid solution after the reaction is finished, carrying out suction filtration on the reaction solution, collecting filter residues, washing the filter residues for 2-4 times, and carrying out vacuum drying to obtain cationic cyclodextrin;
the honeysuckle flavone complex is prepared by taking a honeysuckle flavone extract and metal salt as raw materials and carrying out meridian-collateral reaction;
the complex reaction specifically comprises the following steps:
s1: pulverizing flos Lonicerae, and sieving with 20-40 mesh sieve to obtain flos Lonicerae powder;
s2: adding flos Lonicerae powder into 60-80% ethanol solution at a liquid-material ratio of 1:10-30, placing into an ultrasonic instrument, setting ultrasonic power to 200-300W, extracting at 40-60deg.C for 30-60min for 2-4 times, filtering to obtain residue, mixing extractive solutions, and freeze drying to obtain flos Lonicerae flavone extract;
s3: adding the honeysuckle flavone extract into absolute ethyl alcohol, fully stirring and dissolving, regulating the pH of the solution by using triethylamine, adding metal salt, stirring and mixing, heating to 50-60 ℃, stirring and reacting for 4-12 hours, after the reaction liquid is completely cooled, filtering, separating out a solid product, washing for 2-4 times by using a mixed solution of ethyl alcohol and deionized water, and vacuum drying to obtain the honeysuckle flavone complex.
2. The whitening anti-aging skin brightening liquid according to claim 1, wherein the mass concentration of the sodium hydroxide solution is 20-40%.
3. The whitening anti-aging skin brightening liquid according to claim 1, wherein the mass concentration of the hydrochloric acid solution is 10-15%.
4. The whitening anti-aging skin-brightening liquid according to claim 1, wherein in the step S3, the pH is adjusted to 8-9.
5. The whitening anti-aging skin-brightening liquid according to claim 1, wherein in the step S3, the metal salt is any one of ferric chloride and cupric chloride.
6. The whitening anti-aging skin-brightening liquid according to claim 1, wherein in the step S3, the volume ratio of the ethanol to the deionized water is 1:1.
7. A method for preparing the whitening anti-aging skin-brightening liquid according to any one of claims 1 to 6, which is characterized by comprising the following steps:
SS1: mixing phenethyl resorcinol and a honeysuckle flavone complex, and dissolving the mixture in an ethanol solvent according to a liquid-to-material ratio of 1:5-10 to obtain a premix;
SS2: adding cationic cyclodextrin into deionized water according to a liquid-to-material ratio of 1:10-20, fully stirring to form cationic cyclodextrin aqueous solution, pouring the premixed solution prepared in the step SS1 into the aqueous solution, uniformly mixing, transferring the system into a water bath oscillator, oscillating at a rotating speed of 80-100rpm for 8-12h at a temperature of 20-40 ℃, filtering out precipitate in the solution by using a microporous filter membrane, carrying out vacuum drying, and grinding and crushing the dried product to obtain a cationic cyclodextrin inclusion compound;
SS3: adding deionized water, cationic cyclodextrin clathrate, citrus peel extract, daisy flower extract, radix Pulsatillae extract and glycerol into a high-speed stirrer, stirring uniformly at a rotation speed of 200-500r/min, discharging, and packaging after inspection is qualified to obtain the whitening and anti-aging skin brightening liquid.
8. The method for preparing a whitening anti-aging skin-brightening liquid according to claim 7, wherein in the step SS2, the pore size of the microporous filter membrane is 0.5-3 μm.
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| CN111265463A (en) * | 2020-04-10 | 2020-06-12 | 上海新高姿化妆品有限公司 | Anti-aging cosmetic composition for whitening and brightening skin |
| CN114533644A (en) * | 2022-02-18 | 2022-05-27 | 上海云未生物科技有限公司 | Whitening composition, whitening and freckle-removing essence and preparation method thereof |
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