CN110882192B

CN110882192B - Freckle removing stick and preparation method thereof

Info

Publication number: CN110882192B
Application number: CN201911295061.4A
Authority: CN
Inventors: 袁裕泉; 张娇; 韩志东
Original assignee: Quanhou Guangzhou Research Institute Of Biotechnology Co ltd
Current assignee: Quanhou Guangzhou Research Institute Of Biotechnology Co ltd
Priority date: 2019-12-16
Filing date: 2019-12-16
Publication date: 2021-04-30
Anticipated expiration: 2039-12-16
Also published as: CN110882192A

Abstract

The invention relates to the field of freckle-removing and whitening cosmetics, and provides a freckle-removing stick and a preparation method thereof, wherein the freckle-removing stick comprises the following components in percentage by mass: the component A comprises: the component B is 77.5-87.5: 12.5-22.5; the component A comprises an emollient, an emulsifier, a stabilizer and a humectant; the component B comprises tocopherol, ascorbyl tetraisopalmitate, kojic dipalmitate and Glycyrrhiza glabra root extract; the mass ratio of the tocopherol to the ascorbyl tetraisopalmitate to the kojic acid dipalmitate to the glycyrrhiza glabra root extract is 1.5-3: 3-16: 0.5-8: 0.5-5; the tocopherol, the ascorbyl tetraisopalmitate, the kojic acid dipalmitate and the glycyrrhiza glabra root extract are combined in a specific ratio to obtain a synergistic effect, so that the whitening component has a better effect of penetrating into the skin, a better effect of fading spots and higher safety.

Description

Freckle removing stick and preparation method thereof

Technical Field

The invention relates to the field of freckle-removing and whitening cosmetics, in particular to a freckle-removing stick and a preparation method thereof.

Background

The pigmented spots, which are divided into freckles, dark spots, chloasma, age spots and the like, exist locally or are distributed dispersedly, belong to pigmentary disorder dermatosis, and are common skin diseases with brown or melanosis on the face, which are formed by increasing melanin caused by external ultraviolet rays and other factors, and are frequently generated on cheeks and forehead parts.

At present, a plurality of spot-fading, freckle-removing and whitening products appear on the market, including various whitening masks, essences, whitening creams and the like.

Chinese patent CN 107583183a discloses a three-purpose pen for students to remove acne, macula, and itch, which has the effects of diminishing inflammation, removing acne, blackening, removing macula, and relieving itching and rash, however, the effect of this patent in removing macula is not obvious, and it is easy to soften when making into cream stick, so it is necessary to develop a macula removing stick, which is convenient to use, has remarkable macula removing and whitening effects, and the cream stick has stable appearance, and is suitable for long-term use.

Disclosure of Invention

Aiming at the defects in the prior art, the first purpose of the invention is to provide the spot removing stick which has the advantages of accurate dosage, accurate application on spot parts, low irritation, good spot removing effect and high safety.

In order to achieve the purpose, the invention provides the following technical scheme:

the freckle removing stick comprises the following components in percentage by mass:

the component A comprises: the component B is 77.5-87.5: 12.5-22.5;

the component A comprises an emollient, an emulsifier, a stabilizer and a humectant;

the mass ratio of the emollient to the emulsifier to the stabilizer to the humectant is 41.5-46.5: 10-16: 5-6: 20-22;

the component B comprises tocopherol, ascorbyl tetraisopalmitate, kojic dipalmitate and glycyrrhiza glabra root extract;

the mass ratio of the tocopherol to the ascorbyl tetraisopalmitate to the kojic acid dipalmitate to the glycyrrhiza glabra root extract is 1.5-3: 3-16: 0.5-8: 0.5-5.

The invention is further configured to: the mass ratio of the emollient to the emulsifier to the stabilizer to the humectant is 43-44.5: 11-16: 5-6: 20-21.

The invention is further configured to: the mass ratio of the tocopherol to the ascorbyl tetraisopalmitate to the kojic acid dipalmitate to the glycyrrhiza glabra root extract is (2-3: 6-15): 0.5-4: 0.5-4.5.

The invention is further configured to: the mass ratio of the emollient to the emulsifier to the stabilizer to the humectant is 46.5:16:5: 20.

The invention is further configured to: the mass ratio of the tocopherol to the ascorbyl tetraisopalmitate to the kojic acid dipalmitate to the glycyrrhiza glabra root extract is 2:7.5:0.5: 2.5.

The invention is further configured to: the emollient comprises shea butter and pentaerythritol tetraisostearate, and the mass ratio of the shea butter to the pentaerythritol tetraisostearate is 25-30: 14.5-16.5.

The invention is further configured to: the emulsifier comprises candelilla wax and cetearyl alcohol, and the mass ratio of the candelilla wax to the cetearyl alcohol is 5-11: 5.

The invention is further configured to: the stabilizing agent comprises beeswax and konjac polysaccharide, and the mass ratio of the beeswax to the konjac polysaccharide is 4: 1-2.

The invention is further configured to: the Glycyrrhiza glabra root extract is a glabridin oil solution.

The inventor finds that the tocopherol, the ascorbyl tetraisopalmitate, the kojic acid dipalmitate and the glycyrrhiza glabra root extract are added into the freckle removing stick, and the tocopherol, the ascorbyl tetraisopalmitate, the kojic acid dipalmitate and the glycyrrhiza glabra root extract are combined in a specific ratio to achieve a synergistic effect, so that the whitening component in the freckle removing stick can effectively permeate the base of skin, inhibit the activity of tyrosinase, reduce the formation of melanin, clear free radicals, and can whiten the skin from the root source, so that the whitening component has a better effect of permeating the skin, better spot lightening effect, less possibility of irritation to the skin, and reduction of the probability of red blood streak generation on the skin, and the skin has a substantial whitening and freckle removing effect and higher safety.

The experimental results show that the liquorice glabra root extract can resist aging, has the effect of lightening spots and whitening skin, is matched with tocopherol, ascorbyl tetraisopalmitate and kojic acid dipalmitate in a specific proportion, enables the freckle removing effect of the freckle removing stick to be good, and simultaneously reduces the phenomenon of skin allergy due to the fact that the liquorice glabra root extract and the ascorbyl tetraisopalmitate contain ascorbic acid groups and have irritation to the skin.

The spot-removing stick is added with a humectant and an emollient, wherein the humectant is hydrogenated polyisobutene, and the emollient comprises shea butter and pentaerythritol tetraisostearate, so that the spot-removing stick has a good moisturizing effect, reduces the loss of skin moisture, and well nourishes and protects the skin.

The beewax and the konjac polysaccharide are added into the freckle removing rod to serve as stabilizing agents, the beewax and the konjac polysaccharide are matched in a specific proportion, the stability in the process of preparing the freckle removing rod is improved, a protective film is formed on the outer surface of the freckle removing rod through the konjac polysaccharide, the shape of the freckle removing rod is favorably maintained, the hardness of the prepared freckle removing rod is improved, the condition of softening under a high-temperature condition is reduced, and the freckle removing rod is suitable for being used in tropical regions.

Aiming at the defects in the prior art, the second purpose of the invention is to provide the preparation method of the freckle removing stick, which has the advantages of simple process, low production cost and convenient use of the prepared freckle removing stick.

A preparation method of a freckle removing stick comprises the following steps:

s1, adding an emollient, an emulsifier, a stabilizer and a humectant into an oil bath dissolving tank, heating to 80-90 ℃, keeping for 10-20 min, and uniformly stirring and dissolving to obtain a mixture A;

s2, mixing tocopherol, ascorbyl tetraisopalmitate, kojic acid dipalmitate and glycyrrhiza glabra root extract, and stirring until the mixture is completely dissolved to obtain a solution with the concentration of 10-20% to obtain a mixture B;

s3, preheating the mixture B obtained in the step S2 to 50-60 ℃, slowly dropwise adding the mixture B into the mixture A obtained in the step S1, wherein the volume ratio of the mixture B to the mixture A is 1 (2-4), uniformly mixing, and stirring for 10-30 min at the rotating speed of 300-500 r/min and the water bath temperature of 50-60 ℃ to obtain a uniform solution;

s4, pouring the homogeneous liquid prepared in the step S3 into a lipstick mold, cooling to-25-20 ℃, freezing for 1-2 hours for forming, and demolding to obtain the freckle removing stick.

Compared with the prior art, the invention has the following beneficial effects:

1. according to the invention, the tocopherol, the ascorbyl tetraisopalmitate, the kojic acid dipalmitate and the glycyrrhiza glabra root extract are creatively and reasonably matched together, so that a synergistic effect is obtained, the whitening component has a better effect of penetrating into the skin, the spot fading effect is better, the skin is not easy to be irritated, the skin has a substantial whitening and freckle removing effect, and the safety is higher;

2. according to the freckle removing bar provided by the invention, the beeswax and the konjac polysaccharide are added into the freckle removing bar as the stabilizing agent, and the beeswax and the konjac polysaccharide are matched in a specific ratio, so that the stability in the process of preparing the freckle removing bar is improved, a protective film is formed on the outer surface of the freckle removing bar, the shape of the freckle removing bar is favorably maintained, the hardness of the prepared freckle removing bar is improved, and the condition of softening under a high-temperature condition is reduced;

3. the invention provides a preparation method of a freckle removing stick, which has the advantages of simple process and low production cost, the prepared freckle removing stick is convenient to use, and the prepared freckle removing stick can be accurately smeared on speckle parts.

Drawings

FIG. 1 is a schematic diagram of a product of example 6 of the present invention.

Detailed Description

The present invention will be described in further detail with reference to the accompanying drawings and examples.

In the following examples and comparative examples: the information on the purchasers of the respective raw materials is shown in Table 1.

TABLE 1

Examples 1 to 6, the spot removing stick of the present invention and the preparation method thereof

The formula of the spot removing stick of the embodiment 1-6 is shown in the following table 2.

TABLE 2

The preparation method of the freckle removing stick disclosed by the embodiment 1-6 comprises the following steps:

s1, weighing shea butter, pentaerythritol tetraisostearate, candelilla wax, cetostearyl alcohol, beeswax, konjac glucomannan and hydrogenated polyisobutene, adding into an oil bath dissolving tank, heating to 85 ℃, keeping for 20min, and uniformly stirring for dissolving to obtain a mixture A;

s2, weighing tocopherol, ascorbyl tetraisopalmitate, kojic dipalmitate and glabridin oil solution, adding the solution into deionized water, and stirring until the solution is completely dissolved to obtain a solution with the concentration of 20% as a mixture B;

s3, preheating the mixture B obtained in the step S2 to 60 ℃, and then slowly dropwise adding the mixture B into the mixture A obtained in the step S1, wherein the volume ratio of the mixture B to the mixture A is 1: 4, uniformly mixing, and stirring for 30min at the rotating speed of 500r/min and the water bath temperature of 60 ℃ to obtain a uniform solution;

s4, pouring the homogeneous liquid prepared in the step S3 into a lipstick mold, cooling to-25 ℃, freezing for 2 hours for molding, and demolding to obtain the freckle removing stick as shown in figure 1.

Comparative examples 1 to 5

TABLE 3

As shown in table 3 above:

comparative example 1 differs from example 6 only in that, taking example 6, a whitening cream was prepared, the preparation method comprising the steps of:

a. adding beeswax, shea butter, candelilla wax, hydrogenated polyisobutene, cetostearyl alcohol and pentaerythritol tetraisostearate into a stirring kettle, heating to 85 ℃, and uniformly stirring to obtain a premixed solution;

b. cooling to 65 ℃, adding ascorbyl tetraisopalmitate, kojic acid dipalmitate, glycyrrhiza glabra root extract and tocopherol into the premixed liquid obtained in the step a, and uniformly stirring until the mixture is completely dissolved to form a primary mixed liquid;

c. mixing water, 1, 3-butanediol, EDTA-2Na, tween-20, PEG-20 methyl glucoside sesquistearate, and phenoxyethanol, and heating to 80 deg.C to obtain secondary mixed solution;

d. and (c) pouring the primary mixed liquid prepared in the step (b) into the secondary mixed liquid obtained in the step (c), homogenizing for 3min, stirring and cooling to 35 ℃, and thus obtaining a sample of the emulsified whitening cream.

Comparative example 2 differs from example 6 only in that: comparative example 2 does not contain glabridin oil solution, and the prepared product is a freckle removing stick.

Comparative example 3 differs from example 6 only in that: comparative example 3 does not contain tocopherol and the prepared product is a spot removing bar.

Comparative example 4 differs from example 6 only in that: comparative example 4 does not contain konjac polysaccharide, and the prepared product is a freckle removing stick.

Comparative example 5 differs from example 6 only in that comparative example 5 does not contain beeswax and the product produced is a speckle removing bar.

Test example I, safety test

The skin irritation of the products prepared in examples 1-6 and comparative examples 1-5 was tested according to the skin irritation/corrosion test method of the cosmetic safety specifications 2015, 8 new zealand rabbits were taken from each group, the back hairs of the new zealand rabbits were scraped off, and the skin test skin of the new zealand rabbits was repeatedly applied with spot removing sticks or emulsified whitening creams to determine whether or not there was irritation or corrosion on the local skin of the mammal and the extent thereof, and the test results are shown in table 4 below.

The skin irritation intensity is evaluated by an integral mean value, and the reference indexes are as follows: the integral mean value is 0-0.5 (less than or equal to 0.5) and has no stimulation; slightly stimulating the integration mean value of 0.5-2.0 (less than or equal to 2.0); stimulating in an integral average value of 2.0-6.0 (less than or equal to 6.0); the integral mean value is 6.0-8.0 (less than or equal to 8.0) and strong in irritation.

TABLE 4

As can be seen from the data in table 4, according to the criteria of skin irritation/corrosion test evaluation of the "technical standards for safety of cosmetics" 2015 edition, the multiple skin irritation tests of the freckle removing sticks of examples 1-6 are non-irritating to skin irritation intensity, the multiple skin irritation tests of the whitening cream prepared in comparative example 1 are less irritating to skin, the mass ratio of tocopherol, ascorbyl tetraisopalmitate, kojic dipalmitate and glabridin oil solution in comparative example 1 is within the range protected by examples 1-6, and the freckle removing sticks prepared in comparative example 2 do not contain glabridin oil solution can cause strong irritation to skin, so that the phenomenon of skin allergy can be reduced by utilizing the irritation of the glabrous root extract and the acid groups contained in other components.

The freckle removing stick prepared in the comparative examples 3-5 has no irritation to skin and better safety in multiple skin irritation tests.

Test example two, evaluation of human body irritation

The speckle removing stick or whitening cream prepared in the examples 1-6 and the comparative examples 1-2 is used for carrying out human body irritation test comparison test, and the specific implementation method is as follows:

1) selecting 80 subjects with obvious facial stains, dividing the subjects into 6 groups, and 10 subjects in each group, wherein the subjects clean the whole face;

2) the face of 8 groups of subjects was tested separately for facial mottle, one for each of examples 1-6 and comparative examples 1-2;

3) using for 15 minutes, and self-detecting heat sensation, stabbing pain sensation and redness;

4) the number of people with two different forms of product discomfort was compared as shown in table 5 below.

TABLE 5

Class/number of people	Thermal sensation	Stabbing pain	Redness
				Example 1	1	0	0
Example 2	0	0	0
				Example 3	0	0	0
Example 4	0	0	0
				Example 5	0	0	0
Example 6	0	0	0
				Comparative example 1	1	1	1
Comparative example 2	2	1	2

As can be seen from the data in Table 5, the freckle removing sticks prepared in examples 1-6 have no irritation to skin and mild performance, and the whitening cream prepared in comparative example 1 has less irritation to skin, so that the skin is less irritated and has higher safety when prepared into a stick shape.

The spot removing stick prepared in comparative example 2 lacks glabridin oil solution components, has strong irritation to skin, cannot blend acid groups contained in other components, and has strong irritation.

Test example three, patch test

The test method comprises the following steps: a patch test method for detecting the safety of a human body adopts a 48h closed patch test.

Respectively weighing 20 mu g of the freckle removing sticks prepared in the examples 1 to 6 into a freckle tester, and simultaneously arranging a blank control group which is the basic thinner of the cosmetic. 30 healthy volunteers (students at school) are selected, the age is 20-28 years, and no allergic history exists. After cleaning the back of a subject, the spot tester added with the spot removing stick or whitening cream is pasted on the selected position of the back by using a non-irritating adhesive tape, and the patch is lightly pressed by fingers to be uniformly pasted on the skin for 48 hours after being pasted. The examinee is ordered to keep the spot-pasting part dry within 48h, and violent exercise, scratching the spot-pasting part, long-time sunlight irradiation and the like are avoided. And after 48h, removing the tester and marking, after 30min, judging under sufficient light after the pressure marks disappear, and respectively carrying out revisit observation within 72h and 96 h.

TABLE 6 grading Standard of adverse skin reactions

TABLE 7 adverse skin reaction results

As can be seen from the experimental data in Table 7, the freckle removing sticks prepared in examples 1-6 have no serious adverse reaction, and 30 subjects have no positive reaction, and the results show that the freckle removing sticks prepared in examples 1-6 have no adverse reaction on human bodies.

Similarly, as shown in table 7, it was found through experiments that tocopherol, ascorbyl tetraisopalmitate, kojic dipalmitate, and glycyrrhiza glabra root extract are reasonably mixed together, and the composition is not easy to generate irritation to skin and has high safety.

Test example four measurement of color of skin spots

The purpose of the test is as follows: to verify the stain-lightening effect of the spot-removing stick of the present invention, examples 1 to 6 and comparative examples 1 to 3 were tested.

The test method comprises the following steps: the examples 1-6, the comparative examples 1-3 and the blank examples were used on the pigmented spots of human faces, respectively, the blank example was not treated, 100 persons tested each 10 persons used a sample, and the skin pigmented spots were tested for L (lightness) and b (melanin) using a CK-PMA6CL400 skin tester, skin moisture was tested using a skin moisture tester CM825, skin wrinkles were tested using a skin Rapid three-dimensional imaging System PRIMOS,

l, b, skin moisture and skin wrinkles were measured before and 30 days of use, and the measured L value, b value, skin moisture and average value of skin wrinkles for each sample are shown in Table 8.

Δ L ═ L (after 1 month of the test on the blank or example product) -L (before the start of the test).

Δ b ═ b (before the start of the test) -b (after 1 month of the test on the blank or on the product of the examples).

And subtracting the first detection data from the second detection data of the skin moisture to obtain the change condition of the skin moisture content, wherein the larger the data is, the higher the skin moisture content is.

And subtracting the first detection data from the second detection data of the skin wrinkles to obtain the skin wrinkle change condition, wherein the smaller the data, the fewer the skin wrinkles.

TABLE 8

As can be seen from the data in table 8, the whitening components in examples 1 to 6 have better effect of penetrating into the skin and better effect of lightening spots, wherein the effect of lightening spots is the best with example 6, and more melanin is reduced, so that the skin has substantial whitening and spot removing effects, and the safety is higher.

As can be seen from the data in table 8, the addition of the glabridin oil solution to the freckle removing stick not only can prevent aging, but also has a better speckle lightening effect, and meanwhile, the glabridin oil solution is matched with tocopherol, ascorbyl tetraisopalmitate and kojic acid dipalmitate according to a specific proportion, so that a synergistic effect is obtained, and the freckle removing and whitening effects of the freckle removing stick are better.

Test example five, high temperature Heat resistance measurement of Spot removing stick

The experimental method comprises the following steps: placing a constant temperature incubator in a laboratory, adjusting the temperature of the constant temperature incubator to (50 +/-1) ° c, removing a sleeve of the freckle removing stick prepared in examples 1-6 and comparative examples 4-5, screwing out the freckle removing stick, enabling the freckle removing stick to be vertical to the incubator, detecting the freckle removing stick by using a probe of a flight texture analyzer CT3 millimeter after 24 hours, measuring the hardness of the freckle removing stick by using an ASTM D1321-10 standard method, and when the trigger force of the flight texture analyzer CT3 reaches 5g, enabling the probe to start to penetrate through a sample to a distance of 5 millimeters, wherein the higher the force value is, the higher the sample hardness is, and referring to Table 9.

TABLE 9

As can be seen from the data in table 9, the spot removing sticks prepared in examples 1 to 6 were stable in shape at a temperature of (50 ± 1) ° c, and the hardness of the spot removing sticks was improved, and the phenomenon of flexure due to softening was reduced, while the spot removing sticks prepared in comparative example 4 lack konjac polysaccharide, which indicates that the addition of konjac polysaccharide improves the stability of the spot removing sticks during the preparation process, and helps to maintain the shape of the spot removing sticks.

The freckle removing stick prepared in the comparative example 5 lacks beeswax components, and proves that beeswax and konjac glucomannan are mixed according to a specific proportion, so that the hardness of the freckle removing stick is improved, the phenomenon of bending caused by softening is reduced, and the shape of the freckle removing stick is maintained.

The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.

Claims

1. A freckle removing stick is characterized in that: comprises the following components in percentage by mass:

the component A comprises: the component B is 77.5-87.5: 12.5-22.5;

the component B consists of tocopherol, ascorbyl tetraisopalmitate, kojic dipalmitate and glycyrrhiza glabra root extract;

the mass ratio of the tocopherol to the ascorbyl tetraisopalmitate to the kojic acid dipalmitate to the glycyrrhiza glabra root extract is 1.5-3: 3-16: 0.5-8: 0.5-5;

the emollient comprises shea butter and pentaerythritol tetraisostearate, and the mass ratio of the shea butter to the pentaerythritol tetraisostearate is 25-30: 14.5-16.5;

the emulsifier comprises candelilla wax and cetearyl alcohol, and the mass ratio of the candelilla wax to the cetearyl alcohol is 5-11: 5;

the stabilizing agent comprises beeswax and konjac polysaccharide, and the mass ratio of the beeswax to the konjac polysaccharide is 4: 1-2.

2. The spot removing bar according to claim 1, wherein: the mass ratio of the emollient to the emulsifier to the stabilizer to the humectant is 43-44.5: 11-16: 5-6: 20-21.

3. The spot removing bar according to claim 1, wherein: the mass ratio of the tocopherol to the ascorbyl tetraisopalmitate to the kojic acid dipalmitate to the glycyrrhiza glabra root extract is 2-3: 6-15: 0.5-4: 0.5-4.5.

4. The spot removing bar according to claim 1, wherein: the mass ratio of the emollient to the emulsifier to the stabilizer to the humectant is 46.5:16:5: 20.

5. The spot removing bar according to claim 3, wherein: the mass ratio of the tocopherol to the ascorbyl tetraisopalmitate to the kojic acid dipalmitate to the glycyrrhiza glabra root extract is 2:7.5:0.5: 2.5.

6. The spot removing bar according to claim 1, wherein: the Glycyrrhiza glabra root extract is a glabridin oil solution.

7. The method for preparing a spot removing stick according to any one of claims 1 to 6, wherein the method comprises the following steps: the method comprises the following steps:

s2, mixing tocopherol, ascorbyl tetraisopalmitate, kojic dipalmitate and glycyrrhiza glabra root extract, and stirring until the mixture is completely dissolved to obtain a mixture B;