Acne mark removing essence and preparation method thereof
Technical Field
The invention relates to the technical field of cosmetics, in particular to a novel acne mark removing essence and a preparation method thereof.
Background
It is well known that skin is the weakest part of the body and that daily exposure of human skin presents a number of problems such as acne, acne marks, comedones, pigmentation, sunburn marks, etc. The most common skin diseases are acne, and if a patient is in touch with hands at the affected part during the acne growth period, the patient is not careful about eating, is often in a night, is free to use functional products, is exposed to air pollutants, ultraviolet radiation and the like, a series of skin problems such as acne marks, acne pits, melanin pigmentation, inflammation, oxidative damage, barrier function damage and the like can be caused, the overall facial beauty and the skin state are greatly influenced, and the patient is brought with great psychological stress and even social disorder.
At present, various products with acne mark removing function are developed aiming at the acne mark problem. However, these products may use a large amount of antibiotics, hormones, heavy metals, etc., which are costly, have a large side effect and are toxic. Although the product can effectively inhibit bacteria, resist inflammation and lighten acne marks in a short time, the long-term use of the product can cause the problems of anaphylactic reaction, toxic reaction, inflammatory infection and the like. Thus, many consumers are rapidly increasing in demand for skin care products containing natural ingredients. However, the plant active ingredients have the problems of poor solubility, poor stability, low skin permeability and the like in the application of acne mark removal products, and the application of the plant active ingredients in the acne mark removal products is limited. Fortunately, the nano-carrier technology well solves the problems, greatly expands the application of the plant active ingredients in acne mark removal products, but the existing nano-liposome still has an unstable phenomenon.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a novel acne mark removing essence and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides a novel acne mark removing essence which is characterized by comprising the following components in percentage by mass: 12-18% of a nanostructure lipid carrier, 1.5-3% of a humectant, 0.5-1.2% of an anti-fouling agent, 0.1-0.15% of an anti-allergic agent, 0.1-0.5% of a preservative, 0.5-1% of a pH regulator, 0.01-0.02% of a aromatic agent and the balance of water.
Preferably, the novel acne mark removing essence is characterized in that the nanostructure lipid carrier 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 coating also comprises 3-5% of glycerol monolaurate, 3-5% of calendula oil and 0.5-1% of hydrogel.
Preferably, the hydrogel consists of polyethylene glycol stearate, chitosan, acrylic acid and N, N-methylene bisacrylamide; chitosan in the hydrogel: 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-fouling 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 antiallergic agent is 0.05-0.09% of swertia extract and 0.02-0.07% of coptis extract.
Preferably, the novel acne mark removing essence is characterized in that the preservative is 0.1-0.5% of methylparaben.
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 flavonoids; the chamomile extract comprises flavonoid active ingredients; 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 of:
(1) Preparing a solution containing a Nanostructure Lipid Carrier (NLC): firstly, heating glycerol monolaurate and calendula oil to 50-60 ℃, then adding licorice extract, chamomile extract and grape seed extract into an oil phase, finally, heating a water phase (the water content in the water phase is 40% and the balance of deionized water) of the aqueous gel to 50-60 ℃, and pouring the mixture into the oil phase; further performing ultrasonic treatment on the mixture, and cooling to 25 ℃ to obtain a Nanostructure Lipid Carrier (NLC); and storing it at 4 ℃ for later use;
the hydrogel consists of polyethylene glycol stearate, chitosan, acrylic acid and N, N-methylene bisacrylamide, wherein the chitosan in the hydrogel: polyethylene glycol stearate: acrylic acid: the mass ratio of the N, N-methylene bisacrylamide is as follows: 1:5:15:2, the hydrogel preparation method comprises the following steps: 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 hours, soaking and washing the product with deionized water, drying, and grinding into powder; the acidic solution of the chitosan is a formic acid solution of which the mass fraction is 1% of chitosan or an acetic acid solution of which the mass fraction is 1% of chitosan; the volume mass fraction of the azobisisobutyronitrile in the ethanol solution of the azobisisobutyronitrile is 0.01g/mL; the mass ratio of the azodiisobutyronitrile to the acrylic acid is 0.005-0.02:1;
(2) Preparing acne mark removing essence: firstly adding an anti-allergic agent into 50% of the rest deionized water, stirring for 10-40 min at 60-90 ℃, then adding a humectant and an anti-fouling agent, continuously stirring for 10-40 min, completely dissolving, and cooling to 40-60 ℃; adding the NLC prepared in the step (1) into the NLC, and stirring the NLC at 60-90 ℃ for 10-40 min; and (3) when the temperature is reduced to 35-55 ℃, adding the preservative and the aromatic agent at one time, uniformly stirring, adding the aqueous solution of the pH regulator and the rest deionized water into the essence, regulating the pH value to be 6-6.5, and discharging.
The invention provides an application of the acne mark removing essence or the essence prepared by the preparation method in the technical scheme in acne mark removing.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the novel acne mark removing essence, quercetin and liquorice flavonoids in liquorice extracts can inhibit the activities of tyrosinase and dopachrome tautomerase (TRP-2) and inhibit the polymerization of 5, 6-dihydroxyindole (DHl), so that melanin is prevented from forming, and the effect of whitening skin is achieved.
2. The novel acne mark removing essence prepared by the invention is rich in flavonoid active ingredients, and can remove free radicals and inhibit tyrosinase activity. At the same time, the composition also has antioxidant, antiinflammatory, antiallergic, and antiviral effects.
3. The novel acne mark removing essence prepared by the invention has the advantages that procyanidine contained in grape extract has super-strong antioxidant capacity, collagen is protected, skin elasticity and luster are improved, and whitening, moisturizing and freckle removing effects are realized; reducing wrinkles and keeping skin soft and smooth; can be used for eliminating acne and healing scar.
4. The polysaccharide in the extract contains a plurality of hydrophilic hydroxyl groups, can form hydrogen bonds with water molecules, and can be crosslinked into a net structure so that the novel acne mark removing essence has good water absorbability and moisture retention.
5. According to the novel acne mark removing essence, natural acne mark removing components are added, and assistants such as an anti-fouling agent and a penetration enhancer are added at the same time, so that the essence with a good acne mark removing effect is prepared. Can effectively promote the percutaneous permeation of the plant active ingredients through the nano-carrier technology, 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, thereby preventing the formation of melanin, and promote the catabolism of formed melanin precipitation, so as to achieve the effect of fading acne marks, and the hydrogel on the nano carrier can increase the stability of liposome.
6. According to the preparation method, polyethylene glycol stearate, chitosan, acrylic acid and N, N-methylene bisacrylamide are prepared into hydrogel and are loaded on the outer layer of the nano lipid, wherein the hydrophobic long carbon chain of the polyethylene glycol stearate can be embedded between the liposomes, so that leakage is reduced. The charged repulsive force of the chitosan is beneficial to the stability of liposome and prevents agglomeration; meanwhile, the charge on the surface of chitosan is favorable for combining with cells, and the adsorption capacity is increased. Meanwhile, the polyacrylic acid has excellent water-retaining property.
Drawings
FIG. 1 is a graph showing tyrosinase activity inhibition experiments of examples 1 to 4 and comparative examples 1 to 5;
fig. 2 is a graph showing the penetration of the antiprinting actives into the stratum corneum at various time points for examples 1-4 and comparative examples 1-5.
Description of the embodiments
The present invention is described in detail by the following examples, which are only for further explanation of the present invention and are not to be construed as limiting the scope of the present invention. It is to be understood that various changes and modifications may be made by one skilled in the art after reading the disclosure herein, and that such equivalents are intended to fall within the scope of the claims appended hereto.
Examples 1 to 4:
examples 1 to 4 provide a novel acne mark removing essence which consists of the following components in percentage by weight:
table 1 acne mark removing essence each example content ratio
Note that: in the invention, the balance refers to the defined weight percentage of the components except deionized water in the formula of the essence, and after the contents of all the components in the formula are added, the components are complemented to 100% by deionized water. The essence is daily essence.
It is noted that the nanostructure lipid carrier 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 coating also comprises 3-5% of glycerol monolaurate, 3-5% of calendula oil and 0.5-1% of hydrogel. In the preparation process of the nanostructure lipid carrier, an aqueous phase is required to be added, the mass fraction of the rest water is 40%, and the aqueous solution of the nanostructure lipid carrier is prepared.
The preparation method of the hydrogels of examples 1 to 4 comprises: stirring and dissolving 1g of chitosan in 100mL of acetic acid solution with the mass fraction of 1% in a three-neck flask, adding 5g of polyethylene glycol stearate, adding 15g of acrylic acid into the three-neck flask, stirring and dropwise adding 10mL of azobisisobutyronitrile ethanol solution with the volume mass fraction of 0.01g/mL and 2g of N, N-methylene acrylamide under the protection of nitrogen at the temperature of 50-60 ℃, reacting for 5-8 h, soaking and washing the product with deionized water, drying, and grinding into powder.
The preparation method of the acne mark removing essence of the examples 1-4 comprises the following steps:
(1) Preparing a solution containing a Nanostructure Lipid Carrier (NLC): firstly heating glycerol monolaurate and calendula oil to 55 ℃, then adding licorice extract, chamomile extract and grape seed extract into an oil phase, finally heating an aqueous phase of the aqueous gel (the water content in the aqueous phase is 40% and the balance of deionized water) to 55 ℃, and pouring into the oil phase; further performing ultrasonic treatment on the mixture, and cooling to 25 ℃ to obtain a Nanostructure Lipid Carrier (NLC); and stored at 4 ℃ for later use.
(2) Preparing acne mark removing essence: firstly adding an anti-allergic agent into 50% of the rest deionized water, stirring for 20min at 60-90 ℃, then adding a humectant and an anti-fouling agent, continuously stirring for 20min, completely dissolving, and cooling to 40 ℃; adding the NLC prepared in the step (1) into the NLC, and stirring the mixture at 70 ℃ for 20min; and (3) when the temperature is reduced to 40 ℃, adding the preservative and the aromatic agent at one time, stirring uniformly, adding the aqueous solution of the pH regulator and the rest deionized water into the essence, regulating the pH value to 6.5, and discharging.
Comparative example 1
The novel acne mark removing essence of the comparative example is similar to the preparation method of example 1 in raw materials, and the difference is that: the tremella polysaccharide, grape seed extract and licorice extract were not used.
Comparative example 2
The novel acne mark removing essence of the comparative example is similar to the preparation method of example 1 in raw materials, and the difference is that: the swertia extract, grape seed extract and chamomile extract are not used.
Comparative example 3
The novel acne mark removing essence of the comparative example is similar to the preparation method of the example 1 in raw materials, and the difference is that: the preparation method of the nano-structured lipid carrier (NLC) is that licorice extract, chamomile extract and grape seed extract are added into an aqueous phase, stirring is carried out for 20min at 70 ℃, then humectant and anti-fouling agent are added, stirring is continued for 20min, after complete dissolution, preservative and aromatic are added once when the temperature is reduced to 40 ℃, the aqueous solution of pH regulator and the rest deionized water are added into the essence, the pH value is regulated to 6.5, and discharging is carried out.
Comparative example 4
The novel acne mark removing essence of the comparative example is similar to the preparation method of the example 1 in raw materials, and the difference is that: polyethylene glycol stearate is not added in the preparation process of the hydrogel.
Comparative example 5
The novel acne mark removing essence of the comparative example is similar to the preparation method of the example 1 in raw materials, and the difference is that: chitosan is not added in the preparation process of the hydrogel.
Physical and chemical property test:
the pH value, high-low temperature stability and centrifugal stability of the product are tested to evaluate the physicochemical properties of the product. The pH value of the product is measured by a dilution method by using a pH meter, namely 10.0g of developed anti-acne conditioning essence emulsion is accurately weighed, boiled and cooled deionized water 10.0. 10.0g is added for dilution, the mixture is heated to 40 ℃, the mixture is continuously stirred for uniform dispersion, then the mixture is cooled to room temperature, the corrected pH meter is inserted, the value is read after the reading number is stable, and the average value is measured twice. And (3) testing high and low temperature stability, namely placing the product in a refrigerator at the temperature of minus 15 ℃ for 24 h, taking out, placing in a baking oven at the temperature of 45 ℃ for 24 h, repeating for 3 times, and observing the state of the product.
Physical and chemical property test results:
physical and chemical property tests are carried out on the acne-removing conditioning essence emulsion prepared according to the final formula, the pH value of the acne-removing conditioning essence emulsion is 6.0-6.5, the stability of the acne-removing conditioning essence emulsion is good after high-temperature and low-temperature centrifugation experiments, and no oil-water separation phenomenon is observed.
Irritation test, allergy test:
the hair was cut off from the backs of mice, and the essences prepared in examples 1 to 4 and comparative examples 1 to 5 were respectively applied to the hair-cut portions, and compared with the non-applied portions, and as a result, there were no irritation and anaphylaxis. 1g of the essence obtained in examples 1-4 and comparative examples 1-5 was applied to the surfaces of volunteers, and after 30 minutes, no redness, eruption and foaming occurred.
Acne mark removing essence effect test
Test population: the subjects were all college student volunteers with acne mark problems, including 135 men and women of one to four grades.
Preparation before measurement: the subject's test site was not allowed to use any product (cosmetic or topical) for 3 days prior to the test. Before formal test, the volunteer is subjected to basic test, and after a proper amount of the product is smeared on the ear of the volunteer, whether allergy or other adverse reactions exist or not is observed. Only in all cases, they can sign an informed consent to continue the test.
The testing method comprises the following steps: the test subjects were randomly divided into 9 groups, the trial period was 28 days, the control group samples were applied to the left cheek, the test group samples were applied to the right cheek, and each group was applied once in the morning and evening, each of which was followed once on days 7, 14, 21 and 28, and the same time was followed by the day of the interview, and subjective evaluation data of the subjects were collected.
Evaluation criteria: please 15 subjects per group combined with their own use, the acne mark removal effects of the products of examples 1 to 4 and comparative examples 1 to 5 were scored with the naked eye, and were rated as 4 grades with no effect, no obvious effect, general effect and obvious effect, and the results are shown in table 2:
table 2 acne mark removing essence trial effect
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 examples 1 and 2 are single, the liposome is not present in comparative example 3, and the liposome is not stable in comparative examples 4 and 5 as in examples 1 to 4. Comparative examples 1 to 5 have a smaller inhibitory effect on tyrosinase activity than examples.
In vitro transdermal test: the skin permeability detection was performed on the single use essence for 15 min, 1 h and 2 h respectively in the test area of the subject by using confocal raman technique, so as to obtain the permeation amounts of the anti-imprint active substances in the essence in the stratum corneum at different time points, and the result is shown in fig. 2. It is known that the permeation amount gradually increases as the single use time of the essence is prolonged. Comparative example 3 has low permeation due to the absence of the nano-lipid carrier. Comparative example 4 without polyethylene glycol stearate, comparative example 5 without chitosan, the liposome stability effect was not as good as the example, and the penetration was low.
The comprehensive effect of the essence of the invention is examined
The efficacy of the anti-acne essence prepared in examples 1 to 4 and comparative examples 1 to 5 was evaluated by using trial feeling. The poll evaluation method is adopted to recruit 90 college student volunteers as trial objects, and the college student volunteers are divided into 9 groups, and the essence prepared in examples 1-4 and comparative examples 1-5 are respectively smeared at the acne marks. Twice daily for one month. The total using effects are divided into 10 parts: the score of 10 is the highest score, which shows good and very satisfactory; 8, the method is better; a score of 6 being acceptable; a score of 6 or less is not good and unacceptable. The scoring data for each group was averaged and the results are shown in table 3:
table 3 comprehensive usage 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 skin on the active ingredients. Simultaneously, 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 sediment is promoted, and the effect of fading acne marks is achieved.
The above is only a specific embodiment 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 substantially same technical problems and achieve the substantially same technical effects are encompassed within the scope of the present invention.