Novel acne mark removing essence and preparation method thereof
Technical Field
The invention relates to the technical field of cosmetics, and particularly relates to novel acne mark removing essence and a preparation method thereof.
Background
It is well known that the skin is the weakest part of the body, and the daily exposure of human skin causes many problems, such as acne, acne marks, comedones, pigmentation, sunburn marks, and the like. The most common dermatosis is acne, if a patient touches an affected part with hands, does not pay attention to diet, stays up all night often, uses functional products randomly, is exposed to air pollutants, ultraviolet radiation and the like during acne growing, a series of skin problems such as acne marks, acne pits, melanin pigmentation, inflammation, oxidation damage, barrier function damage and the like can be caused, the whole facial beauty and skin state are greatly influenced, great psychological pressure is brought to the patient, and even social disorder is caused.
At present, various products with acne mark removing function have been developed aiming at the problem of acne marks. However, these products may use a large number of antibiotics, hormones, heavy metals, etc. which are costly, have significant side effects and are toxic. Although the product can effectively inhibit bacteria, resist inflammation and reduce acne marks when used in a short time, the product can cause the problems of anaphylactic reaction, toxic reaction, inflammatory infection and the like when used for a long time. Thus, the demand of skin care products containing natural ingredients is rapidly increasing by many consumers. However, the plant active ingredients have the problems of poor solubility, poor stability, low skin permeability and the like in the application of the acne mark removing product, so that the application of the plant active ingredients in the acne mark removing product is limited. Fortunately, the problems are well solved by the nano-carrier technology, the application of the plant active ingredients in the acne mark removing product is greatly expanded, but the existing nano-liposome still has an unstable phenomenon.
Disclosure of Invention
In order to solve the problems, the invention aims to provide novel acne mark removing essence and a preparation method thereof.
In order to solve the technical problem, the technical scheme adopted by the invention is as follows:
the invention provides novel acne mark removing essence which is characterized by comprising the following components in percentage by mass: 12 to 18 percent of nano-structured lipid carrier, 1.5 to 3 percent of humectant, 0.5 to 1.2 percent of anti-fouling agent, 0.1 to 0.15 percent of anti-allergic agent, 0.1 to 0.5 percent of preservative, 0.5 to 1 percent of pH regulator, 0.01 to 0.02 percent of aromatic and the balance of water.
Preferably, the novel acne mark removing essence is characterized in that the nanostructured lipid carrier is 0.5-3% of liquorice extract, 1-5% of chamomile extract and 1-5% of grape seed extract; according to the mass percentage, the toothpaste also comprises 3 to 5 percent of glycerol monolaurate, 3 to 5 percent of calendula oil and 0.5 to 1 percent of hydrogel.
Preferably, the hydrogel is composed of polyethylene glycol stearate, chitosan, acrylic acid and N, N-methylene bisacrylamide; the hydrogel comprises chitosan: polyethylene glycol stearate: acrylic acid: the mass ratio of the N, N-methylene-bisacrylamide is as follows: 1:5:15:2.
Preferably, the novel acne mark removing essence is characterized in that the humectant is 0.5-1.5% of hyaluronic acid and 0.5-1.2% of tremella polysaccharide.
Preferably, the novel acne mark removing essence is characterized in that the anti-pollution agent comprises 0.03-0.09% of vitamin C, 0.01-0.08% of vitamin E and 0.4-1% of ferulic acid.
Preferably, the novel acne mark removing essence is characterized in that the anti-allergic agent is 0.05-0.09% of swertia herb extract and 0.02-0.07% of coptis chinensis extract.
Preferably, the novel acne mark removing essence is characterized in that the preservative is 0.1-0.5% of methyl hydroxybenzoate.
Preferably, the novel acne mark removing essence is characterized in that the pH regulator is triethanolamine 0.5-1%.
Preferably, the novel acne mark removing essence is characterized in that the licorice extract comprises quercetin and licorice flavonoid; the chamomile extract contains a flavonoid active ingredient; the grape seed extract comprises procyanidins.
The invention also provides a preparation method of the novel acne mark removing essence, which is characterized by comprising the following steps:
(1) Preparation of a solution containing Nanostructured Lipid Carriers (NLC): firstly, heating glycerol monolaurate and calendula oil to 50-60 ℃, then adding a liquorice extract, a chamomile extract and a grape seed extract into an oil phase, and finally heating a water phase containing hydrogel (the water content in the water phase is 40 percent of the rest deionized water) to 50-60 ℃, and pouring the water phase into the oil phase; further subjecting the mixture to ultrasonic treatment, cooling to 25 deg.C to obtain Nanostructured Lipid Carrier (NLC); and storing it at 4 ℃ for later use;
the hydrogel is composed of polyethylene glycol stearate, chitosan, acrylic acid and N, N-methylene bisacrylamide, and the ratio of chitosan: polyethylene glycol stearate: acrylic acid: the mass ratio of the N, N-methylene bisacrylamide is as follows: 1: adding an acidic solution of chitosan, polyethylene glycol stearate and acrylic acid into a three-neck flask, stirring and dropwise adding an ethanol solution of azodiisobutyronitrile and N, N-methylene acrylamide at the temperature of 50-60 ℃ under the protection of nitrogen, reacting for 5-8 h, soaking and washing a product with deionized water, drying, and grinding into powder; the acid solution of the chitosan is a formic acid solution with the mass fraction of 1% of chitosan or an acetic acid solution with the mass fraction of 1% of chitosan; the volume mass fraction of the azodiisobutyronitrile in the ethanol solution of the azodiisobutyronitrile is 0.01g/mL; the mass ratio of the azodiisobutyronitrile to the acrylic acid is 0.005-0.02;
(2) Preparing acne mark removing essence: firstly, adding the anti-allergic agent into 50 percent of the rest deionized water, stirring for 10-40 min at 60-90 ℃, then adding the humectant and the anti-fouling agent, continuously stirring for 10-40 min, and cooling to 40-60 ℃ after complete dissolution; adding the NLC prepared in the step (1) into the mixed solution, and stirring the mixed solution for 10 to 40min at a temperature of between 60 and 90 ℃; when the temperature is reduced to 35-55 ℃, the preservative and the aromatic are added at one time, the mixture is stirred evenly, the aqueous solution of the pH regulator and the rest deionized water are added into the essence together, the pH value is adjusted to 6-6.5, and the material is discharged.
The invention provides application of the acne mark removing essence in the scheme or the essence prepared by the preparation method in the technical scheme in the acne mark removing.
Compared with the prior art, the invention has the beneficial effects that:
1. in the novel acne mark removing essence prepared by the invention, quercetin and licorice flavonoids in the licorice extract can inhibit the activity of tyrosinase and dopachrome tautomerase (TRP-2) and inhibit the polymerization of 5,6-dihydroxyindole (DHl) so as to prevent the formation of melanin, thereby achieving the effect of whitening skin.
2. According to the novel acne mark removing essence prepared by the invention, the chamomile extract is rich in flavonoid active ingredients, and can be used for removing free radicals and inhibiting tyrosinase activity. At the same time, the composition has antioxidant, anti-inflammatory, antiallergic, and antiviral effects.
3. According to the novel acne mark removing essence prepared by the invention, procyanidine contained in the grape extract has super-strong oxidation resistance, collagen is protected, the elasticity and luster of skin are improved, and whitening, moisturizing and freckle removing effects are achieved; reducing wrinkles and keeping the skin smooth; removing acne and healing scar.
4. According to the novel acne mark removing essence prepared by the invention, the polysaccharide in the extract contains a plurality of hydrophilic hydroxyl groups, and can form hydrogen bonds with water molecules and be mutually crosslinked into a network structure, so that the novel acne mark removing essence shows good water absorption and moisture retention.
5. According to the novel acne mark removing essence prepared by the invention, natural acne mark removing components are added, and auxiliary agents such as an anti-fouling agent and a penetration enhancer are added to prepare the essence with a good acne mark removing effect. The nano-carrier technology can effectively promote the percutaneous permeation of the plant active ingredients and remarkably increase the retention of the active ingredients by the skin. Meanwhile, the nano-carrier can effectively improve the solubility of insoluble active ingredients, enhance the stability of the active ingredients, realize the synergistic inhibition of tyrosinase by various active ingredients, prevent the formation of melanin and promote the catabolism of formed melanin precipitates, thereby achieving the effect of lightening acne marks, and the hydrogel on the nano-carrier can improve the stability of the liposome.
6. The invention is prepared by preparing the polyethylene glycol stearate, the chitosan, the acrylic acid and the N, N-methylene bisacrylamide into hydrogel which is loaded on the outer layer of the nano liposome, wherein the hydrophobic long carbon chain of the polyethylene glycol stearate can be embedded between the liposomes, thereby reducing leakage. The repulsion of charges carried by the chitosan is beneficial to the stability of the liposome and the prevention of agglomeration; meanwhile, the electric charge carried on the surface of the chitosan is beneficial to being combined with cells, and the adsorption capacity is increased. Meanwhile, polyacrylic acid has excellent water retention.
Drawings
FIG. 1 is a graph showing tyrosinase activity inhibition experiments in examples 1 to 4 and comparative examples 1 to 5;
fig. 2 is a graph of the permeation of the marking-removing active in the stratum corneum at different points in time for examples 1 to 4 and comparative examples 1 to 5.
Detailed Description
The present invention is described in detail below with reference to examples, which are provided for further illustration of the present invention and are not to be construed as limiting the scope of the present invention. It should be understood that various changes and modifications can be made by those skilled in the art after reading the disclosure of the present invention, and equivalents fall within the scope of the appended claims.
Examples 1 to 4:
embodiments 1 to 4 provide a novel acne mark removing essence, which comprises the following components in percentage by weight as shown in table 1:
table 1 acne mark removing essence in each example
Note: in the invention, the balance refers to the components except deionized water in the formula of the essence, wherein the components have limited weight percentage content, and after the contents of all the components in the formula are added, the deionized water is finally used for complementing to 100%. The essence is daily essence.
It is noted that the nanostructured lipid carrier of the invention is 0.5-3% of licorice extract, 1-5% of chamomile extract and 1-5% of grape seed extract; according to the mass percentage, the toothpaste also comprises 3 to 5 percent of glycerol monolaurate, 3 to 5 percent of calendula oil and 0.5 to 1 percent of hydrogel. In the preparation process of the nano-structure lipid carrier, a water phase is required to be added, wherein the mass fraction of the water is 40% of the balance, and the water solution of the nano-structure lipid carrier is prepared.
The preparation method of the hydrogel of the embodiment 1 to 4 comprises the following steps: 1g of chitosan is stirred and dissolved in 100mL of acetic acid solution with the mass fraction of 1 percent in a three-neck flask, 5g of polyethylene glycol stearate is added, 15g of acrylic acid is added into the three-neck flask, 10mL of azodiisobutyronitrile ethanol solution with the volume fraction of 0.01g/mL and 2g of N, N-methylene acrylamide are stirred and dripped under the protection of nitrogen at the temperature of 50-60 ℃, and after reaction for 5-8 hours, the product is soaked and washed by deionized water, dried and ground into powder.
The preparation method of the acne mark removing essence of embodiments 1 to 4 includes the following steps:
(1) Preparation of a solution containing Nanostructured Lipid Carriers (NLC): firstly, heating glycerol monolaurate and calendula oil to 55 ℃, then adding a liquorice extract, a chamomile extract and a grape seed extract into an oil phase, finally heating a water phase containing hydrogel (the water content in the water phase is 40 percent of the rest deionized water) to 55 ℃, and pouring the water phase into the oil phase; further subjecting the mixture to ultrasonic treatment, cooling to 25 deg.C to obtain Nanostructured Lipid Carrier (NLC); and stored at 4 ℃ until use.
(2) Preparing acne mark removing essence: firstly, adding the anti-allergic agent into 50 percent of the rest deionized water, stirring for 20min at the temperature of 60-90 ℃, then adding the humectant and the anti-fouling agent, continuously stirring for 20min, and cooling to 40 ℃ after complete dissolution; adding the NLC prepared in the step (1) into the mixture, and stirring the mixture for 20min at 70 ℃; cooling to 40 deg.C, adding antiseptic and aromatic, stirring, adding the aqueous solution of pH regulator and the rest deionized water into the essence, adjusting pH to 6.5, and discharging.
Comparative example 1
The raw materials and the preparation method of the novel acne mark removing essence are similar to those in example 1, and the differences are that: the tremella polysaccharide, grape seed extract and licorice extract were not used.
Comparative example 2
The raw materials and the preparation method of the novel acne mark removing essence are similar to those in example 1, and the difference is that: the swertia extract, grape seed extract and chamomile extract were not used.
Comparative example 3
The raw materials and the preparation method of the novel acne mark removing essence are similar to those of example 1, and the difference is that: the preparation method of the nano-structured lipid carrier (NLC) is not adopted, and comprises the steps of adding a liquorice extract, a chamomile extract, a grape seed extract and an anti-allergy agent into a water phase, stirring for 20min at 70 ℃, then adding a humectant and an anti-fouling agent, continuously stirring for 20min, cooling to 40 ℃ after complete dissolution, adding a preservative and an aromatic once, uniformly stirring, adding the water solution of a pH regulator and the rest deionized water into an essence, adjusting the pH value to 6.5, and discharging.
Comparative example 4
The raw materials and the preparation method of the novel acne mark removing essence are similar to those of example 1, and the difference is that: polyethylene glycol stearate is not added in the preparation process of the hydrogel.
Comparative example 5
The raw materials and the preparation method of the novel acne mark removing essence are similar to those of example 1, and the difference is that: the preparation process of the hydrogel does not add chitosan.
And (3) testing physical and chemical properties:
and testing the pH value, the high and low temperature stability and the centrifugal stability of the product to evaluate the physical and chemical properties of the product. The pH value of the product is measured by a dilution method and a pH meter, wherein 10.0g of the developed acne-removing conditioning essence milk is accurately weighed, 10.0g of boiled and cooled deionized water is added for dilution, the mixture is heated to 40 ℃, stirring is continuously carried out during the period to uniformly disperse the mixture, then the mixture is cooled to room temperature, a corrected pH meter is inserted, the numerical value is read after the reading is stable, and the average value is obtained by measuring twice. And (3) testing the high and low temperature stability, namely placing the product in a refrigerator at the temperature of 15 ℃ below zero for 24 hours, taking out the product, placing the product in an oven at the temperature of 45 ℃ for 24 hours, repeating the steps for 3 times, and observing the state of the product.
Physical and chemical property test results:
the physical and chemical performance test is carried out on the acne-removing conditioning essence emulsion prepared according to the final formula, the pH value is 6.0-6.5, the stability is good after high-low temperature and centrifugal experiments, and no oil-water separation phenomenon is observed.
Irritation test, allergy test:
the back of the mice was cut to remove hairs, and the essences prepared according to examples 1 to 4 and comparative examples 1 to 5 were applied to the cut-to-hair parts, respectively, and compared with the non-applied parts, no irritation or allergic reaction was observed. 1g of the essence obtained in the examples 1 to 4 and the comparative examples 1 to 5 is smeared on the surface of a volunteer hand, and no redness, rash or blister phenomenon appears after 30 minutes.
Acne mark removing essence effect test
Testing the population: subjects were college student volunteers with acne marks problem, including 135 men and women of one to four years.
Preparation before measurement: the subject site was not allowed to use any product (cosmetic or topical drug) within 3 days prior to the trial. Before formal test, the basic test is carried out on the volunteers, a proper amount of the product is smeared on the ears of the volunteers, and whether allergy or other adverse reactions exist is observed. Only in all cases successfully can they sign an informed consent to continue to participate in the test.
The test method comprises the following steps: the test period is 28 days, the samples of the control group are smeared on the left cheek, the samples of the test group are smeared on the right cheek, each group is smeared once in the morning and at the evening, the groups are respectively followed up once on the 7 th day, the 14 th day, the 21 st day and the 28 th day, the following up days are the same time, and the subjective evaluation data of the testee are collected.
And (4) judging the standard: each group of 15 subjects was asked to visually grade the acne mark removing effects of the products of examples 1 to 4 and comparative examples 1 to 5 in combination with their own use conditions, and the results were ranked 4 times in total, namely, ineffective, unobvious, general and obvious effects, as shown in table 2:
TABLE 2 trial effect of acne mark removing essence
|
Invalid (human)
|
Unobvious effect (human)
|
Effect in general (human)
|
Obvious effect (human)
|
Total effective rate (%)
|
Example 1
|
1
|
1
|
3
|
10
|
93.3
|
Example 2
|
2
|
2
|
2
|
9
|
86.7
|
Example 3
|
2
|
1
|
4
|
8
|
86.7
|
Example 4
|
1
|
1
|
3
|
10
|
93.3
|
Comparative example 1
|
4
|
1
|
4
|
6
|
73.3
|
Comparative example 2
|
3
|
3
|
3
|
6
|
80.0
|
Comparative example 3
|
5
|
2
|
3
|
5
|
66.7
|
Comparative example 4
|
3
|
1
|
4
|
7
|
80.0
|
Comparative example 5
|
2
|
3
|
4
|
6
|
86.7 |
The tyrosinase activity inhibition experimental method comprises the following steps: T/SHRH 015, the experimental results are shown in FIG. 1. It can be seen that the acne mark removing components in comparative example 1 and comparative example 2 are single, no liposome is present in comparative example 3, and the liposome is less stable than in comparative examples 1 to 4 in comparative example 4 and comparative example 5. Comparative examples 1 to 5 were inferior to examples in tyrosinase activity inhibitory effect.
In vitro transdermal test: by utilizing a confocal Raman technology, the skin permeability detection is carried out on the skin after 15min, 1h and 2h of the single-use essence in the test area of the testee, so as to obtain the permeation amount of the mark-removing active substances in the essence in the stratum corneum at different time points, and the result is shown in figure 2. It can be seen that the amount of penetration gradually increases with the increase of the single use time of the essence. Comparative example 3 the permeation amount was low due to the absence of the nano lipid carrier. Comparative example 4 without polyethylene glycol stearate and comparative example 5 without chitosan, the liposome stability effect was not as good as the examples, and the penetration was low.
The invention discloses the inspection of comprehensive effect of essence
The effects of the acne mark removal essences prepared in examples 1 to 4 and comparative examples 1 to 5 were evaluated by using a trial feeling. 90 college student volunteers were recruited as trial subjects by adopting a civil survey evaluation method, divided into 9 groups, and the essence prepared in examples 1 to 4 and comparative examples 1 to 5 were applied to the acne marks. It is administered twice daily for one month. The total using effect of each item is 10 points: 10 points are the highest points, which represent good and very satisfactory; 8 is preferably divided into; 6 is acceptable; when the score is 6 or less, it is not preferable and is not acceptable. The score data for each group were averaged and the results are shown in table 3:
TABLE 3 comprehensive use effects
In conclusion, the essence prepared by the invention can effectively promote the percutaneous permeation of the plant active ingredients and remarkably increase the retention of the active ingredients in the skin. Meanwhile, the solubility of insoluble active ingredients is effectively improved, the stability of the active ingredients is enhanced, and the synergistic inhibition of tyrosinase by various active ingredients is realized, so that the formation of melanin is prevented, the catabolism of formed melanin precipitates is promoted, and the effect of lightening the acne marks is achieved.
The above are only specific embodiments of the present invention, but the technical features of the present invention are not limited thereto. Any simple changes, equivalent substitutions or modifications made on the basis of the present invention to solve the same technical problems and achieve the same technical effects are all covered in the protection scope of the present invention.