CN113081903A - Transparent whitening essence containing 4-butylresorcinol and preparation method thereof - Google Patents

Abstract

The invention relates to the technical field of cosmetics, in particular to transparent whitening essence containing 4-butyl resorcinol, which comprises water, a thickening agent, a humectant, a preservative, a solubilizer, a fat-imparting agent and 4-butyl resorcinol, aims to solve the water-solubility problem of the 4-butyl resorcinol applied to the cosmetics, provides a reasonable collocation of raw materials and a content range of the 4-butyl resorcinol, prepares the 4-butyl resorcinol which is originally insoluble in water into the transparent essence, and has good efficacy and appearance.

Description

Transparent whitening essence containing 4-butylresorcinol and preparation method thereof

Technical Field

The invention relates to the technical field of cosmetics, in particular to transparent whitening essence containing 4-butyl resorcinol and a preparation method thereof.

Background

The search for whitening raw materials in the cosmetic industry has never been stopped, and meanwhile, whitening is a constant pursuit of oriental women, but consumers need to take effect quickly for whitening, while the traditional whitening raw materials need 1-2 months, so that the consumers do not have the patience in use. As a result, consumers' growing appetite is met only by providing products that quickly achieve whitening effects.

In the last decades, resorcinol derivatives have been found to have a very strong potential whitening effect, and have the advantages of fast whitening speed, interest of consumers, in-vitro experiments also prove that the resorcinol derivatives are tens of times or even hundreds of times stronger than VC, the whitening capability of the resorcinol derivatives is clinically proved to be comparable to that of hydroquinone, and through continuous understanding of the properties and safety of the raw materials for more than ten years, the resorcinol derivatives gradually obtain the permission of each country at present and are gradually used in cosmetics.

For example, resorcinol includes phenylethyl resorcinol (dezhi 377, a patent product, belonging to cosmetic limited substances), dimethoxytolyl-4-propyl resorcinol (a main active ingredient in the same patent product as that of CL-302), 4-butyl resorcinol, and the like.

Of these, 4-butylresorcinol is a white to off-white crystalline powder, soluble in most organic solvents, slightly soluble in water, and has a melting point of about 50 ℃. 4-butyl resorcinol has been proved to inhibit the generation of melanin, the activity of tyrosinase and TRP-1, inhibit the synthesis of tyrosinase by directly inhibiting the activity of tyrosinase and B16 melanoma cells, and do not cause any cytotoxicity, and meanwhile, the risk factor of 4-butyl resorcinol in cosmetics and skin care products is safe, so that the skin can be relieved and wrinkled, namely, the skin types of 5. It can be used for pregnant women without influence and acne, and 4-butylresorcinol is suitable for tolerant skin, pigmented skin, non-pigmented skin, and oily skin

Upon a search of the prior art disclosures, the inventors,

the publication technology 1-CN 106924108B discloses a whitening and freckle-removing cream, wherein 2 whitening components of 4-butylresorcinol and glabridin are reasonably compatible with an ultraviolet absorbent (ethylhexyl methoxycinnamate) and moisturizing and anti-wrinkle components (sodium hyaluronate, biological carbohydrate gum-1 and hydroxydecyl ubiquinone) in a cream formula, so that stimulation of excessive ultraviolet radiation to skin is reduced, melanin formation is prevented, the skin is effectively protected, and excellent whitening, freckle-removing and moisturizing effects are achieved.

The publication technology 2-CN111743851B discloses a whitening and spot-lightening composition and application thereof, wherein the whitening and spot-lightening composition comprises the following raw materials: egg yolk oil, shea butter, pterostilbene, vitamin E, hydrolyzed ceramide III, orange peel extract, yeast extract, thyme extract, white willow bark extract, mullein extract, lilium maritimum nerve activity whitening factor, scutellaria baicalensis extract, oxyresveratrol, lactobacillus fermentation lysate, tranexamic acid, VC ethyl ether, water-soluble fullerene, 4-butylresorcinol, and ectoin; and the application of the whitening and spot-lightening composition in cosmetics.

The defects of the prior art are combined as follows:

(1) the disclosed technology 1 is to apply 4-butyl resorcinol to a cosmetic cream emulsifying system, and does not solve the problem of applying the raw material to transparent essence;

(2) the disclosed technology 2 is only a simple physical mixing of various active ingredients having whitening and spot-lightening effects, and also does not mention a specific method of solving the problem of water solubility of 4-butylresorcinol.

Disclosure of Invention

Aiming at the existing problems, the invention aims to solve the water solubility problem of 4-butyl resorcinol applied to cosmetics and provide a transparent whitening essence containing 4-butyl resorcinol, which can still keep transparent appearance when applied to an aqueous solution system of the cosmetics.

The technical purpose of the invention is realized by the following technical scheme that the transparent whitening essence containing 4-butyl resorcinol comprises the following components in parts by weight,

water 100

0.1-1.0 part of thickening agent

Humectant 5.0-10.0

0.5-3.0% of preservative

0.1-0.5 of solubilizer

Fat-imparting agent 2.0-10.0

4-butyl resorcinol 0.1-0.5.

According to the invention, through reasonable matching of the raw materials and the content range of the 4-butyl resorcinol, the 4-butyl resorcinol which is originally insoluble in water is prepared into the transparent essence, and the transparent essence has good efficacy and appearance.

Preferably, the thickener is at least one of polyacrylate cross-linked polymer-6, transparent xanthan gum, sodium hyaluronate, sodium polyglutamate, hydroxyethyl cellulose, carrageenan, tara gum and sodium polyacrylate.

Preferably, the humectant is at least one of glycerin, propylene glycol, butylene glycol, dipropylene glycol, isopropanol and trehalose.

Preferably, the preservative is at least one of 1, 2-pentanediol, p-hydroxyacetophenone, 1, 2-hexanediol, caprylic hydroxamic acid, phenoxyethanol and glyceryl caprylate.

Preferably, the solubilizer is at least one of PEG-40 hydrogenated castor oil, LRI, SP-115C, HPS.

Further preferably, the LRI comprises PPG-26-Butaneth-26, PEG-40 hydrogenated castor oil and water, and the manufacturer is Senxin, Germany.

Further preferably, the SP-115C comprises water, PEG-50 hydrogenated castor oil, nonylphenol polyether-14, and propylene glycol, and is manufactured by Shanghai Cippon Biotech Co.

Further preferably, the HPS comprises Coco polyether-7, PPG-1-PEG-9 lauryl glycol ether and PEG-40 hydrogenated castor oil, which was manufactured by Pasteur Germany.

Preferably, the fat-endowing agent is PEG-6 caprylic acid/capric acid triglyceride and/or PEG-8 caprylic acid/capric acid triglyceride

The invention also provides a preparation method of the transparent whitening essence containing 4-butyl resorcinol, which comprises the following steps:

s1: mixing humectant and 4-butyl resorcinol, stirring, and heating to completely transparent;

s2: adding a solubilizer, water and a fat-imparting agent into the liquid prepared in the step S1, and stirring until the liquid is completely transparent;

s3: adding a thickening agent into the liquid prepared in the step S2, heating to 80-85 ℃, stirring until the thickening agent is completely dissolved, and cooling;

s4: and (5) cooling the solution prepared in the step (S3) to below 40 ℃, adding a preservative, and uniformly stirring to obtain the transparent whitening essence.

In conclusion, the invention has the following beneficial effects:

firstly, in the thickener used in the invention, polyacrylate cross-linked polymer-6 can be used as a film forming agent, sodium hyaluronate is a component of skin and some tissues of human body, and is the best natural moisturizing component for skin, so that the moisture in tissue cells can be maintained, and the maintenance can not be lost due to the amount of ambient moisture, and sodium polyglutamate enables the product of the invention to have extremely strong moisturizing capability and promotes the health of skin.

Secondly, the risk coefficient of 1, 2-pentanediol in the preservative used by the invention is 1, the preservative is safe and can be used safely, the preservative generally has no influence on pregnant women, and the 1, 2-pentanediol has no acne-causing property, the p-hydroxyacetophenone is a mild, additive-free and non-irritant preservative, has the functions of antioxidation and sedation and relief, has a synergistic effect when being compounded with other preservatives, and the caprylyl hydroximic acid is compatible with most raw materials, is not influenced by the raw materials such as surfactants, proteins and the like in a receptor system, and can be compounded with the preservatives such as alcohols and glycols;

thirdly, the solubilizer is PEG-40 hydrogenated castor oil or other three large-scale enterprise raw materials, so that on one hand, the raw materials of the product are convenient to obtain, and on the other hand, the product batch difference of the three enterprises is stable due to the fact that the product needs to be accurately controlled, and the batch production of the product is facilitated;

fourthly, the whitening essence containing 4-butyl resorcinol is effectively ensured to be transparent in appearance through a scientific and reasonable preparation method.

Drawings

Fig. 1 is a result of a whitening efficacy test of examples and comparative examples.

Detailed Description

The present invention is described in further detail below with reference to examples, which are intended to facilitate the understanding of the present invention and are not intended to limit the present invention in any way. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.

The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.

The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.

When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.

The transparent whitening essence containing 4-butyl resorcinol comprises 100 parts of water, 0.1-1.0 part of thickening agent, 5.0-10.0 parts of humectant, 0.5-3.0 parts of preservative, 0.1-0.5 part of solubilizer, 2.0-10.0 parts of fat-imparting agent and 0.1-0.5 part of 4-butyl resorcinol.

Explanation of the respective raw materials:

the thickener is at least one of polyacrylate cross-linked polymer-6, transparent xanthan gum, sodium hyaluronate, sodium polyglutamate, hydroxyethyl cellulose, carrageenan, Caesalpinia spinosa gum and sodium polyacrylate;

the humectant is at least one of glycerol, propylene glycol, butanediol, dipropylene glycol, isopropanol, and trehalose;

the antiseptic is at least one of 1, 2-pentanediol, p-hydroxyacetophenone, 1, 2-hexanediol, caprylyl hydroxamic acid, phenoxyethanol and glyceryl caprylate;

the solubilizer is at least one of PEG-40 hydrogenated castor oil, LRI and SP-115C, HPS;

wherein, the LRI comprises PPG-26-butanol polyether-26, PEG-40 hydrogenated castor oil and water, and is from Germany forest jasmine;

wherein, the SP-115C comprises water, PEG-50 hydrogenated castor oil, nonylphenol polyether-14 and propylene glycol, and is from Shanghai Xinpu Biotech limited;

wherein the HPS comprises Coco polyether-7, PPG-1-PEG-9 lauryl glycol ether and PEG-40 hydrogenated castor oil, and is derived from Pasteur Germany;

the fat-imparting agent is PEG-6 caprylic acid/capric acid triglyceride and/or PEG-8 caprylic acid/capric acid triglyceride.

Inventive examples 1 to 5 and comparative examples 1 to 5 were compared, and the contents of the respective components are shown in the following table 1,

TABLE 1 statistical table of raw material component contents of each example

The "/" part above indicates that this material was not added. The humectant A is butanediol, the humectant B is trehalose, the thickener A is transparent xanthan gum, the thickener B is sodium hyaluronate, the preservative A is p-hydroxyacetophenone, the preservative B is 1, 2-hexanediol, the fat-imparting agent is PEG-8 caprylic/capric triglyceride, and the solubilizer is HPS produced by Pasteur.

The above examples 1 to 5 and comparative examples 1 to 5 were each prepared as follows,

s1: mixing humectant and 4-butyl resorcinol, stirring, and heating to completely transparent;

s2: adding a solubilizer, water and a fat-imparting agent into the liquid prepared in the step S1, and stirring until the liquid is completely transparent;

s3: adding a thickening agent into the liquid prepared in the step S2, heating to 80-85 ℃, stirring until the thickening agent is completely dissolved, and cooling;

s4: and (6) cooling the solution prepared in the step (S3) to below 40 ℃, adding a preservative, and uniformly stirring to obtain the whitening essence.

Results of the experiment

First, appearance inspection

The whitening essences prepared in examples 1 to 5 and comparative examples 1 to 5 were each placed in the same transparent bottle, and observed to have the following structure in table 2 below,

TABLE 2 appearance of examples 1-5 and comparative examples 1-5

As can be seen from Table 2, in examples 1-5, the humectant, the fat-imparting agent and the solubilizer are included in spite of different proportions of the components, so that 4-butylresorcinol can be well dissolved in water to form a transparent system. In contrast, comparative examples 1-5, which lacked a single starting material to varying degrees, resulted in a material body that was milky in appearance, indicating that 4-butylresorcinol was not well solubilized in water, resulting in an opaque milky appearance.

Second, test of whitening effect

1. Test method

1) Test products: examples 1-5, comparative examples 1-5;

2) testing the population: 100 persons;

3) age: between 20-35 years old;

4) the test requirements are as follows: the test sample can be used regularly according to requirements in a matched test, and any other whitening product can not be used in the test period;

5) testing an instrument: multifunctional skin tester MPA6, germany CK company, Mexameter MX18 melanin and heme test probe;

6) the test method and the judgment standard are as follows: the designated area of the face of the testee was used as the test area, 100 persons were divided into 10 groups corresponding to examples 1-5 and comparative examples 1-5, respectively, the MPA6 skin tester was used together with Mexameter MX18 melanin and heme test probes to test the change of melanin content of the skin on days 1, 7, 14 and 28 after the start of the experiment, and the average value of 10 persons in each group was counted for each test.

2. Test results

Referring specifically to fig. 1, examples 1 to 5 gradually enhanced the whitening effect as the content of 4-butylresorcinol increased, whereas comparative examples 1 to 5 significantly reduced the whitening effect because 4-butylresorcinol was not completely dissolved in water and did not well permeate into the skin.

Third, safety evaluation test

1. Test method-evaluation by human body patch test

The subjects were counted for 30 persons, and the specific gender and age were determined at random (meeting the inclusion and exclusion criteria of "diagnostic criteria and treatment principles for cosmetic contact dermatitis"). The samples prepared in examples 1-5 were placed in a plaque tester (sample amount 0.020-0.025 g), a blank containing no substance was taken, the sample and blank were applied to the curved side of the forearm of the subject, and the sample and blank were applied to the skin by gentle pressure with the palm for 24 hours. And (5) after the spot tester is removed for 30min, observing skin reaction after the indentation disappears. If the result is negative, the observation is performed once more at 24h and 48h respectively.

The criteria for classification and judgment according to "diagnostic criteria and treatment principles for cosmetic contact dermatitis" are shown in Table 3. The judgment standard is that the number of people with grade 1 adverse skin reactions is more than 5, the number of people with grade 2 adverse skin reactions is more than 2, or any grade 1 adverse skin reactions, grade 3 adverse skin reactions or more than 3 adverse skin reactions occur in 30 subjects after the patch test is carried out for 24 hours, and the subjects are judged to have adverse skin reactions on human bodies.

TABLE 3 diagnostic score criteria for cosmetic contact dermatitis

3. The result of the detection

The results of the patch test are shown in table 4:

TABLE 4 test results of human body patches

According to the statistics shown, the transparent whitening essence containing 4-butyl resorcinol prepared in the examples 1-5 has no adverse reaction on human skin after the patch test.

In summary, it is known from the appearance that examples 1 to 5 can make 4-butyl resorcinol, which is difficult to dissolve in water, completely dissolve in water and completely transparent by reasonable matching of raw materials. Examples 1 to 5 all had significant whitening effect and were excellent in completeness. Among them, the effect of example 5 is particularly excellent.

The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is conceivable, and the examples presented herein demonstrate the results of applicants' actual experiments. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.

Claims (10)

1. The transparent whitening essence containing 4-butyl resorcinol is characterized by comprising the following components in parts by weight,

water 100

0.1-1.0 part of thickening agent

Humectant 5.0-10.0

0.5-3.0% of preservative

0.1-0.5 of solubilizer

Fat-imparting agent 2.0-10.0

4-butyl resorcinol 0.1-0.5.

2. The transparent whitening essence according to claim 1, wherein the thickener is at least one of polyacrylate cross-linked polymer-6, transparent xanthan gum, sodium hyaluronate, sodium polyglutamate, hydroxyethyl cellulose, carrageenan, tara gum and sodium polyacrylate.

3. The transparent whitening essence of claim 1, wherein the humectant is at least one of glycerin, propylene glycol, butylene glycol, dipropylene glycol, isopropyl alcohol, and trehalose.

4. The transparent whitening essence of claim 1, wherein the preservative is at least one of 1, 2-pentanediol, p-hydroxyacetophenone, 1, 2-hexanediol, caprylyl hydroxamic acid, phenoxyethanol, and glyceryl caprylate.

5. The transparent whitening essence of claim 1, wherein the solubilizing agent is at least one of PEG-40 hydrogenated castor oil, LRI, SP-115C, HPS.

6. The essence of claim 5, wherein the LRI comprises PPG-26-Butanethol-26, PEG-40 hydrogenated castor oil and water, and the manufacturer is Doffy.

7. The transparent whitening essence of claim 5, wherein the SP-115C comprises water, PEG-50 hydrogenated castor oil, nonylphenol polyether-14, and propylene glycol, and is manufactured by Shanghai Xinpu Biotech limited.

8. The whitening serum of claim 5, wherein the HPS comprises Coco polyether-7, PPG-1-PEG-9 lauryl glycol ether and PEG-40 hydrogenated castor oil, which are manufactured by Pasteur Germany.

9. The transparent whitening essence of claim 1, wherein the fatting agent is PEG-6 caprylic/capric triglyceride and/or PEG-8 caprylic/capric triglyceride.

10. A preparation method of a transparent whitening essence containing 4-butylresorcinol is characterized by comprising the following steps:

s1: mixing humectant and 4-butyl resorcinol, stirring, and heating to completely transparent;

s2: adding a solubilizer, water and a fat-imparting agent into the liquid prepared in the step S1, and stirring until the liquid is completely transparent;

s3: adding a thickening agent into the liquid prepared in the step S2, heating to 80-85 ℃, stirring until the thickening agent is completely dissolved, and cooling;

s4: and (5) cooling the solution prepared in the step (S3) to below 40 ℃, adding a preservative, and uniformly stirring to obtain the transparent whitening essence.

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