Colloidal sulfur-based acne-removing composition as well as preparation method and application thereof

Abstract

The invention relates to the technical field of skin external preparations, in particular to a colloidal sulfur-based acne-removing composition and a preparation method and application thereof.The colloidal sulfur-based acne-removing composition is at least prepared from, by weight, 10-50 parts of colloidal sulfur, 3-12 parts of ethyl lauroyl arginate hydrochloride, 3-12 parts of palmitoyl proline, 10-50 parts of glycolipid, 3-20 parts of kaolin, 3-12 parts of panthenol and 3-12 parts of o-cymene-5-ol. Colloidal sulfur is introduced to be compounded with specific bioactive components to prepare the composition capable of efficiently resisting acnes, removing blackheads, resisting inflammation and repairing barriers, and the composition can be subsequently added into face cleansing products for synergism.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of skin external preparation, in particular to a colloidal sulfur-based acne-removing composition, a preparation method and application thereof. BACKGROUND

[0002] There are many acne-removing and blackhead-removing products in the market, but they all have the following problems: sulfur preparations are unstable (traditional sulfur is easy to oxidize and deteriorate, has strong irritation, has a large odor, and has low bioavailability), single components have limitations (salicylic acid and peroxides are prone to cause dryness and desquamation, and cannot balance antibacterial and barrier repair), and mineral fillers have single function (ordinary kaolin only has physical adsorption, and lacks synergistic active ingredient design). A crystalline oil-controlling acne-removing multi-functional amino acid facial cleanser and a preparation method thereof are disclosed in Chinese Patent Application (Publication No. CN116712345A), which realizes self-thickening effect by optimizing the compounding and ratio of amino acid salt and sodium stearoyl glutamate in the system, and overcomes the shortcomings of existing thickening agents and pH regulators in product stability and use experience, but the acne-removing and blackhead-removing effects of the product need to be further improved. SUMMARY

[0003] To solve the above problems, the present application provides a colloidal sulfur-based acne-removing composition, a preparation method and application thereof, which introduces colloidal sulfur and specific bioactive ingredients to prepare a composition with high efficiency in anti-acne, blackhead removal, anti-inflammatory and barrier repair, and the composition can be added to a facial cleanser for synergistic effect.

[0004] In one aspect, the present application provides a colloidal sulfur-based acne-removing composition, which comprises at least, by weight: 10-50 parts of colloidal sulfur, 3-12 parts of lauroyl arginine ethyl ester hydrochloride, 3-12 parts of palmitoyl proline, 10-50 parts of glycolipid, 3-20 parts of kaolin, 3-12 parts of panthenol, and 3-12 parts of o-cymen-5-ol.

[0005] In one embodiment, the composition comprises at least, by weight: 20-40 parts of colloidal sulfur, 5-10 parts of lauroyl arginine ethyl ester hydrochloride, 5-10 parts of palmitoyl proline, 20-40 parts of glycolipid, 5-10 parts of kaolin, 5-10 parts of panthenol, and 5-10 parts of o-cymen-5-ol.

[0006] In one embodiment, the colloidal sulfur is in a protective colloidal state bridged by gum arabic, and the elemental sulfur maintains its S8 polygonal structure.

[0007] In one embodiment, the kaolin satisfies at least one of the following conditions:

[0008] (1) the pH is neutral;

[0009] (2) the spatial structure is laminated;

[0010] (3) the mass ratio of magnesium to ferric oxide is 0.2-0.1: 60-58.

[0011] In an embodiment, the glycolipid is a bio-fermented polysaccharide type structural glycolipid.

[0012] The present application provides a composition including colloidal sulfur, lauroyl arginine ethyl ester hydrochloride, palmitoyl proline, glycolipid, kaolin, panthenol, o-cymen-5-ol, which can effectively improve the oil control effect of the product when applied to a subsequent cleansing system. Further, by optimizing the ratio of colloidal sulfur, lauroyl arginine ethyl ester hydrochloride, palmitoyl proline, glycolipid, kaolin, panthenol, and o-cymen-5-ol, the product can improve the anti-acne, blackhead removal, anti-inflammatory, and barrier repair effects of the product when applied to a subsequent cleansing system without affecting the foam performance of the cleansing product.

[0013] The present application provides a preparation method of a colloidal sulfur-based acne-removing composition, which at least includes the following steps: mixing colloidal sulfur, PCA lauroyl arginine ethyl ester salt, palmitoyl proline, and kaolin to obtain a mixture; and adding panthenol, o-cymen-5-ol, and glycolipid to the mixture under stirring.

[0014] The present application provides a use of a colloidal sulfur-based acne-removing composition in the preparation of a cleansing product, and the addition amount of the colloidal sulfur-based acne-removing composition in the cleansing product is 0.1-50 wt%.

[0015] In an embodiment, the addition amount of the colloidal sulfur-based acne-removing composition in the cleansing product is 0.1-20 wt%.

[0016] In an embodiment, the cleansing product includes at least one of a cleansing milk, a cleansing foam, a cleansing mousse, a cleansing jelly, a cleansing soap, a cleansing cream, a cleansing lotion, a cleansing powder, and a cleansing oil.

[0017] In an embodiment, the preparation raw material of the cleansing product at least includes a colloidal sulfur-based acne-removing composition, potassium cocoate, potassium palmitate, potassium oleate, a plant extract, sodium cocoyl methyl taurate, lauryl hydroxy sultaine, a thickening agent, polyquaternium-39, and polyquaternium-7.

[0018] In an embodiment, the plant extract is at least one of a calendula extract, a wild soybean extract, a lemon extract, a hamamelis virginiana extract, or a mint extract.

[0019] In an embodiment, the thickening agent at least includes hydroxypropyl methylcellulose and an acrylic acid (ester) copolymer.

[0020] The mass ratio of the hydroxypropyl methyl cellulose, acrylic acid (ester) copolymer is (0.1-0.2):(2-3).

[0021] In an embodiment, the preparation raw materials of the facial cleanser product include, by weight parts, 2-12 parts of the colloidal sulfur-based acne-removing composition, 30-50 parts of potassium cocoate, 10-30 parts of potassium palmitate, 0.5-1.5 parts of potassium oleate, 0.02-2 parts of plant extract, 5-12 parts of sodium cocoyl methyl taurate, 2-10 parts of lauryl hydroxysultaine, 1-4 parts of thickening agent, 0.5-1.5 parts of polyquaternium-39, and 0.5-1.5 parts of polyquaternium-7.

[0022] The colloidal sulfur-based acne-removing composition provided by the present application can be added to any facial cleanser system for synergistic effect, has good compatibility with raw materials such as surfactants in the facial cleanser system, and ensures excellent stability of the product.

[0023] The colloidal sulfur-based acne-removing composition provided by the present application is convenient to use, simple in preparation method, stable in performance, and easy to realize large-scale industrial production and popularization and application.

[0024] Advantages

[0025] 1. The present application provides a colloidal sulfur-based acne-removing composition, a preparation method and application thereof, which is prepared by introducing colloidal sulfur and specific bioactive ingredients to prepare a composition with high efficiency in anti-acne, blackhead removal, anti-inflammatory and barrier repair, and can be subsequently added to a facial cleanser for synergistic effect.

[0026] 2. The present application designs the composition to include colloidal sulfur, lauroylethylarginate hydrochloride, palmitoyl proline, glycolipid, kaolin, panthenol and o-cymen-5-ol, so that the product provided can effectively improve the oil control effect when applied to a facial cleanser system subsequently.

[0027] 3. The present application optimizes the ratio of colloidal sulfur, lauroylethylarginate hydrochloride, palmitoyl proline, glycolipid, kaolin, panthenol and o-cymen-5-ol, so that the product provided can improve the anti-acne, blackhead removal, anti-inflammatory and barrier repair effects when applied to a facial cleanser system subsequently without affecting the foam performance of the facial cleanser.

[0028] 4. The colloidal sulfur-based acne-removing composition provided by the present application can be added to any facial cleanser system for synergistic effect, has good compatibility with raw materials such as surfactants in the facial cleanser system, and ensures excellent stability of the product.

[0029] 5. The colloidal sulfur-based acne-removing composition provided by the present application is convenient to use, simple in preparation method, stable in performance, and easy to realize large-scale industrial production and popularization and application. BRIEF DESCRIPTION OF DRAWINGS

[0030] Figure 1 The stability test results of the products provided for application examples 1, 4, 6 are shown in the figure, the left side of the figure is the sample of application example 1, the middle is the sample of application example 4, and the right side is the sample of application example 6.

[0031] Figure 2 The stability test results of the products provided for application comparative examples 1, 4, 6 are shown in the figure, the left side of the figure is the sample of application comparative example 1, the middle is the sample of application comparative example 4, and the right side is the sample of application comparative example 6.

[0032] Figure 3 The appearance of the material of the products provided for application example 1 and application comparative example 9 is shown in the figure, the left side of the figure is the sample of application example 1, and the right side is the sample of application comparative example 9. The lower figure is an enlarged view of the upper figure.

[0033] Figure 4 The ISGA score results of application example 1 and the blank control.

[0034] Figure 5 The acne lesion count results of application example 1 and the blank control.

[0035] Figure 6 The local acne-removing effect comparison chart of application example 1 and the blank control is shown in the figure, the left side of the figure is the blank control, and the right side is application example 1.

[0036] Figure 7 The local blackhead-removing effect comparison chart of application example 1 and the blank control is shown in the figure, the left side of the figure is the blank control, and the right side is application example 1. DETAILED DESCRIPTION

[0037] The raw material information in the various embodiments, comparative examples, application examples, and application comparative examples of the present application is as follows:

[0038] 1. Colloidal sulfur (Sulfidal Colloidal Sulfur Cosmetic Grade): Aurorium Company, USA

[0039] 2. Lauric arginine ethyl ester hydrochloride (HONDU LAE-200): Guangzhou Hongdu Fine Chemicals

[0040] 3. Palmitoyl proline (HONDU DP-95S): Guangzhou Hongdu Fine Chemicals

[0041] 4. Sugar lipid (RHEANCE One): Wacker Chemical

[0042] 5. Kaolin (GOLD & RED CLAY): BERACA-CLARIANT

[0043] 6. Ubiquinol (D-ubiquinol): DSM

[0044] 7. Isopropylmethylphenol: Osaka Kagaku

[0045] 8. Potassium cocoate, potassium palmitate, potassium oleate (NAFOCLEA DCB-45H, NAFOCLEA DCB-40M): Hongdu Chemical

[0046] 9. Sodium cocoyl methyl taurate (HONDU CT-30DS): Hongdu Chemical

[0047] 10. Lauryl hydroxysultaine (AMPHITOL 20HD): Shanghai Huakang

[0048] 11. Hydroxypropyl methylcellulose (HPMC 40-0202): DOW Chemical

[0049] 12. Acrylate copolymer (Carbopol Aqua SF-1): Lubrizol

[0050] 13. Polyquatemium-39 (Merquat Plus 3330 Polymer): Lubrizol

[0051] 14. Polyquatemium-7 (Merquat 740 polymer): Lubrizol

[0052] 15. Soybean oil and Calendula officinalis flower extract (Calendula Oil CLR): Germany CLR.

[0053] Examples 1-10, Comparative Examples 1-10

[0054] Examples 1-10, Comparative Examples 1-10 of the present application provide, on a weight basis, a colloidal sulfur-based acne-removing composition, the formulation of which is shown in Table 1 and Table 2.

[0055] Table 1

[0056]

[0057]

[0058] Table 2

[0059]

[0060] The colloidal sulfur is in a protective colloidal state bridged by gum arabic, while the elemental sulfur maintains its S8 polygonal structure. The high clay satisfies the following conditions simultaneously: (1) pH is neutral; (2) space structure is laminated; (3) mass ratio of magnesium to ferric oxide is 0.2-0.1:60-58. The glycolipid is a biologically fermented polysaccharide type glycolipid.

[0061] Embodiments 1-10 of the present application provide, in another aspect, a method for preparing a colloidal sulfur-based acne-removing composition, comprising the following steps: mixing colloidal sulfur, PCA cocoyl ethyl amine salt, palmitoyl proline, and high clay under stirring to obtain a mixture; and adding panthenol, o-cymen-5-ol, and glycolipid into the mixture under stirring.

[0062] Comparative Examples 1-10 of the present application provide, in another aspect, a method for preparing a colloidal sulfur-based acne-removing composition, comprising the following steps: mixing the raw materials according to the formula table under stirring.

[0063] Application Examples 1-10 and Comparative Examples 1-10

[0064] Application Examples 1-10 and Comparative Examples 1-10 of the present application provide a cleansing cream containing a colloidal sulfur-based acne-removing composition. The formula is shown in Table 3 and Table 4.

[0065] Table 3

[0066]

[0067] Table 4

[0068]

[0069]

[0070] Performance test

[0071] 1. Oil control rate test

[0072] The cleansing cream samples provided by the application examples and comparative examples are configured into 10 wt% aqueous solution, and a bubble maker is used to make the solution fully foamed. The foam is applied to the forehead cleaning range of the tester, gently massaged for 30 seconds, and then washed with water. The Sebumeter SM815 skin oil test probe is used to test the initial skin oil content of the volunteers (i.e. before cleaning with the cleansing cream) and the skin oil content 3 hours after washing (the smaller the measured value, the lower the skin surface oil content). The oil control rate is calculated, and the results are shown in Table 5.

[0073] Table 5

[0074]

[0075] From the analysis of Table 5, it can be seen that the cleansing creams provided by the application examples 1-10 have better oil control effect than the cleansing creams provided by the application comparative examples 1-10.

[0076] 2. Foam performance test

[0077] Using the Ross Foam Tester, using deionized water, the cleansing cream samples provided by the application examples and the application comparative examples are configured into a 0.5wt% aqueous solution, placed in a water bath at 40℃±0.5 for incubation, the Ross Foam Tester is used to test the foam height of the product, and the "initial foam height" and the "end foam height" after 15 minutes are recorded, and the foam height retention rate% = end foam height / initial foam height*100% is calculated, and the test results are shown in Table 6.

[0078] Table 6

[0079]

[0080] From the analysis of Table 6 data, it can be seen that the cleansing creams provided by the application examples 1-10 have better foam height retention rate than the cleansing creams provided by the application comparative examples 1-10.

[0081] 3. Physical properties

[0082] (1) Stability test: The stability of the cleansing cream provided by the present application is tested, and the test results are shown in Table 7-Table 8 and Figures 1-2 .

[0083] Table 7 Stability test results of application examples 1, 4, 6

[0084]

[0085] Table 8 Stability test results of application comparative examples 1, 4, 6

[0086]

[0087]

[0088] (2) Material appearance: The material appearance of the application example 1 and the application comparative example 9 are compared (see Figure 3 ), from the appearance, it can be seen that the comparative example 9 has uneven black particles, the pearl luster is not delicate, and there are a small amount of non-uniformly dispersed components, while the material of the example 1 is uniform, the pearl luster is delicate and has layers.

[0089] (3) Viscosity (25℃) and material smearing property, foam stickiness test, the results are shown in Table 9, in Table 9, the more "★", the better the material smearing property; the more "★", the less sticky the foam.

[0090] Table 9

[0091]

[0092] 4. Acne and blackhead removal ability test

[0093] Test method: 30 min after facial cleansing, use VISIA-CR facial image analyzer to take pictures of the face, and use IPP software (image analysis software Image-Pro Plus 7.0) to analyze the proportion of acne lesion area and lesion color a* value in the area of interest (AOI), then apply application example 1 and blank control (the specific formula is the same as application example 1, without adding colloidal sulfur-based acne-removing composition) and guide the use method, the subjects return 14 days after using the product and conduct the same index detection, and the test results are as follows.

[0094] (1) ISGA score, a dermatologist evaluates the acne lesion on the face of the subject before and after the subject uses the product. The ISGA scale is used to score the improvement of the lesion before and after the subject uses the product, and the percentage of lesion reduction is calculated (percentage of lesion reduction = (ISGA score before using the product - ISGA score after using the product) / ISGA score before using the product x 100%), by comparing the ISGA scores before and after use, the acne-removing effect of the product can be reflected, and the results are shown in Table 9 and Table 10. Figure 4

[0095] Table 10

[0096] Product control ISGA score p-value (vs. D0) Blank control 2.03±0.53 / Application Example 1 1.45±0.56 <0.01

[0097] Analysis of Table 10 and Table 11 Figure 4 The results show that compared with the blank control group, the ISGA lesion score of application example 1 shows a downward trend after using the product, and the percentage of lesion reduction after use is 28.57%, which has a very significant difference (p < 0.01).

[0098] (2) Acne lesion count (pimple, papule and pustule)

[0099] The dermatologist counts the number of facial lesions (pimple, papule, pustule) of the subject before and after the subject uses the product, and calculates the percentage of lesion number reduction. By comparing the change of lesion number before and after use, the acne-removing effect of the product can be reflected (the more the number of facial acne lesions decreases, the better the improvement effect of acne lesions, indicating that the acne-removing effect of the product is better), and the results are shown in Table 11 and Table 12. Figure 5 Figure 6 The results of blackhead removal are shown in Table 13. Figure 7

[0100] The change rate of the number of pimples = (the number of pimples after using the product - the number of pimples before using the product) / the number of pimples before using the product x 100%.​​​

[0101] The rate of change in the number of papules = (the number of papules after use - the number of papules before use) / the number of papules before use x 100%;

[0102] The rate of change in the number of papules = (the number of papules after use - the number of papules before use) / the number of papules before use x 100%.

[0103] (3) The results of the ability to remove acne and blackheads are summarized in Table 11.

[0104] Table 11

[0105]

[0106] 5. Virulence test

[0107] (1) Test method: The experimental animals were examined within 24 hours before the start of the test. Animals with eye irritation symptoms, corneal defects, and conjunctival damage were not used in the test. On the day of the test, the lower eyelid of one eye of the experimental animal was gently pulled open, and 0.1 m of the test substance (a 10 wt% aqueous solution prepared from the preparation of Example 1) was dropped into the conjunctival sac, and the upper and lower eyelids were passively closed for 1 second to prevent the test substance from being lost. The other eye was not treated as a self-control. The eyes were not rinsed within 24 hours after the test substance was dropped. The animal's eyes were examined at 1, 24, 48, 72 hours after the test substance was dropped, and on the 4th day and the 7th day. If there is no irritation reaction within 72 hours, the test can be terminated. Eye irritation examination can be performed using a magnifying glass, a hand-held slit lamp, a biological microscope, or other instruments and equipment used. After the 24-hour observation and recording is completed, further examination is performed on the eyes of all animals using fluorescein sodium. In each examination, the eye irritation score should be recorded according to the scoring criteria for eye damage in Table 1 of Chapter 6, 5 Acute Eye Irritation / Corrosion Test, of the Cosmetic Safety Technical Specification (2015 Edition). The mean value of the irritation score of the cornea, iris, or conjunctiva of the animal after being given the test substance at the 24, 48, 72-hour observation time points and the recovery time are evaluated, and the irritation intensity of the test substance to the eye is determined according to Table 2 of Chapter 6, 5 Acute Eye Irritation / Corrosion Test, of the Cosmetic Safety Technical Specification (2015 Edition).

[0108] (2) Test results: During the observation period, none of the three animals showed any irritation reaction, as shown in Table 12.

[0109] Table 12

[0110]

[0111] Note: The integral mean refers to the mean of the stimulation response integral of the animal's cornea, iris or conjunctiva at 24, 48 and 72 hours after the test substance.

[0112] From the above table, it can be seen that the mean of the stimulation response integral of the animal's cornea, iris or conjunctiva at 24, 48 and 72 hours after the test substance (concentration 10wt%) is 0, according to the raw material eye irritation response grading standard of Chapter 6 5 Acute Eye Irritation / Corrosion Test of the Cosmetic Safety Technical Specification (2015 Edition), it belongs to non-irritation.

Claims

1. A colloidal sulfur-based acne treatment composition characterized in that, At least comprising, by weight parts: colloidal sulfur 10-50 parts, lauroyl ethyl arginate hydrochloride 3-12 parts, palmitoyl proline 3-12 parts, glycolipid 10-50 parts, kaolin 3-20 parts, panthenol 3-12 parts, o-cymen-5-ol 3-12 parts.

2. The colloidal sulfur-based acne treatment composition of claim 1, wherein, At least comprising, by weight parts: colloidal sulfur 20-40 parts, lauroyl ethyl arginate hydrochloride 5-10 parts, palmitoyl proline 5-10 parts, glycolipid 20-40 parts, kaolin 5-10 parts, panthenol 5-10 parts, o-cymen-5-ol 5-10 parts.

3. The colloidal sulfur-based acne treatment composition of claim 1, wherein, The kaolin satisfies at least one of the following conditions, (1) pH is neutral; (2) the space structure is laminated; (3) the mass ratio of magnesium to ferric oxide is 0.2-0.1:60-58.

4. A process for the preparation of a colloidal sulfur-based acne treatment composition according to any one of claims 1 to 3, characterized in that, At least comprising the following steps: mixing colloidal sulfur, PCA ethyl lauroyl arginate salt, palmitoyl proline, kaolin to obtain a mixture; adding panthenol, o-cymen-5-ol, glycolipid to the mixture under stirring.

5. Use of a colloidal sulfur-based acne treatment composition according to any one of claims 1 to 3, characterized in that, Applied to the preparation of a facial product, the addition amount of the colloidal sulfur-based acne-removing composition in the facial product is 0.1-50wt%.

6. Use of a colloidal sulfur-based acne treatment composition according to claim 5, characterized in that, The facial product comprises one of facial milk, facial foam, facial mousse, facial jelly, facial soap, facial cream, facial lotion, facial powder, and facial oil.

7. Use of a colloidal sulfur-based acne treatment composition according to claim 5, wherein The preparation raw materials of the facial product at least comprise a colloidal sulfur-based acne-removing composition, potassium laurate, potassium palmitate, potassium oleate, plant extract, sodium cocoyl methyl taurate, lauryl hydroxysultaine, thickening agent, polyquaternium-39, and polyquaternium-7.

8. Use of a colloidal sulfur-based acne treatment composition according to claim 7, characterized in that, The plant extract is at least one of calendula extract, wild soybean extract, lemon extract, hamamelis virginiana extract, or mint extract.

9. Use of a colloidal sulfur-based acne treatment composition according to claim 7, wherein The thickening agent at least comprises hydroxypropyl methyl cellulose and acrylic acid (ester) copolymer.

10. Use of a colloidal sulfur-based acne treatment composition according to claim 7, wherein The preparation raw materials of the facial product at least comprise, by weight parts, 2-12 parts of a colloidal sulfur-based acne-removing composition, 30-50 parts of potassium laurate, 10-30 parts of potassium palmitate, 0.5-1.5 parts of potassium oleate, 0.02-2 parts of plant extract, 5-12 parts of sodium cocoyl methyl taurate, 2-10 parts of lauryl hydroxysultaine, 1-4 parts of thickening agent, 0.5-1.5 parts of polyquaternium-39, and 0.5-1.5 parts of polyquaternium-7.

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