Salicylic acid-coated oil-control acne-removal composition and preparation method thereof

Abstract

The invention provides a salicylic acid-coated oil-control acne-removal composition and a preparation method thereof, and belongs to the field of cosmetic compositions. The preservative comprises the following components: salicylic acid, macadamia oil, salvia oil, a wrapping wall material, sodium dihydrogen phosphate and sodium hydroxide. The salicylic acid and the skin care essential oil are wrapped and microencapsulated by adopting the composite wall material, and the porous structure of the wall material can delay the release speed of the salicylic acid; in addition, the fat-soluble core material (containing macadamia oil) is combined with the hydrophilic wall material, so that salicylic acid can penetrate through an epidermis grease layer to directly reach hair follicles, and the cutin barrier cannot be damaged due to excessive permeation; finally, the effects of prolonging the action time and reducing stimulation are achieved.

Description

Technical Field

[0001] The present invention belongs to the field of cosmetic compositions, and in particular relates to an oil-controlling and acne-removing composition encapsulating salicylic acid and a preparation method thereof. Background Art

[0002] Salicylic acid is a common skincare ingredient. It's fat-soluble and can penetrate deep into pores to dissolve oil and unclog sebaceous glands, effectively controlling oil and removing acne, inhibiting the growth of Propionibacterium acnes, and reducing the appearance of blackheads. It also promotes keratin metabolism, improves rough, dull skin, and alleviates inflammatory skin conditions. It can also brighten the skin tone, fade acne scars, and enhance the absorption of other active ingredients. However, it can be highly irritating and can easily cause dryness, peeling, or sensitivity, requiring gradual tolerance building from low concentrations. Furthermore, it carries the risk of photosensitivity, necessitating strict sun protection after use.

[0003] The core approaches to reducing the irritation of salicylic acid focus on material encapsulation, formulation optimization, and bioengineering technology. Through supramolecular encapsulation techniques (such as molecular aggregates formed with cyclodextrin, gum arabic, or poloxamer) or liposome / microsphere encapsulation, salicylic acid can be slowly released, reducing peak concentrations upon direct contact with the skin while extending its duration of action and maintaining stability at low pH values (2.5-3.8).

[0004] Formula optimization reduces acidic corrosiveness by adjusting the pH value (such as using alkaline neutralizers or buffer systems), and compounding soothing ingredients such as ceramides and panthenol to repair the barrier.

[0005] In the field of bioengineering, microbial fermentation or enzyme catalysis technology (such as genetically modified strains that efficiently convert raw materials) is used to replace traditional chemical synthesis, reducing by-products and irritating impurities. At the same time, green processes such as supercritical fluid extraction or ultrasonic-assisted extraction are developed to reduce the risk of solvent residues. Summary of the Invention

[0006] The first object of the present invention is to provide an oil-control and acne-removing composition encapsulating salicylic acid, comprising the following components in parts by mass:

[0007]

[0008]

[0009] Preferably, the wrapping wall material comprises at least one of the following components:

[0010] Hydroxypropyl cyclodextrin, cyclodextrin, gum arabic.

[0011] More preferably, the wrapping wall material is a mixture of hydroxypropyl cyclodextrin, cyclodextrin, and gum arabic, with a mass ratio of 20-25:15-20:3-5.

[0012] A second object of the present invention is to provide a method for preparing the aforementioned oil-control and acne-removing composition encapsulated with salicylic acid, comprising the following steps:

[0013] S1 Core material pre-emulsification: Salicylic acid, Australian blue cedar oil, and sage oil are mixed and dissolved in ethanol; sodium dihydrogen phosphate is then added to adjust the pH to 5.0-6.5, and shear emulsification is performed to form a core material emulsion;

[0014] S2 wall material solution preparation: dissolve the wrapped wall material in water; then add sodium hydroxide to adjust the solution pH to 8.0-9.0 to form a wall material solution with a solid content of 30-40%;

[0015] S3 microencapsulation: the core material emulsion and the wall material solution are mixed, and then homogenized into a uniform emulsion and dried to obtain an oil-controlling and anti-acne composition encapsulating salicylic acid.

[0016] Preferably, in the core material pre-emulsification step S1, the shear emulsification temperature is ≤60°C, and the amount of ethanol used is at least twice the mass of salicylic acid.

[0017] Preferably, in the preparation of the S2 wall material solution, the temperature of the wall material solution is 60-80°C.

[0018] A third object of the present invention is to provide the use of the aforementioned salicylic acid-encapsulated oil-control and acne-removing composition in the preparation of cosmetics; cosmetics include creams, essences, lotions, facial masks, toners, or cleansers. The salicylic acid-encapsulated oil-control and acne-removing composition is present in a leave-on cosmetic at a minimum weight percentage of 1%.

[0019] The present invention uses composite wall materials to encapsulate salicylic acid and skin care essential oil ingredients into microencapsulated form. The porous structure of the wall material can slow the release rate of salicylic acid. In addition, the fat-soluble core material (containing Australian blue cedar oil) is combined with the hydrophilic wall material, allowing salicylic acid to penetrate the epidermal oil layer directly to reach the hair follicles without damaging the keratin barrier due to excessive penetration, ultimately achieving the effect of prolonging the action time and reducing irritation.

[0020] In terms of effect, salicylic acid unclogs pores by dissolving keratin plugs, while Australian blue cypress oil and sage oil provide antibacterial and anti-inflammatory auxiliary effects, forming a dual-effect system of "acne removal and oil control". DETAILED DESCRIPTION

[0021] In order to better understand the present invention, the present invention is further described below in conjunction with specific serial numbers, wherein the terms used in the serial numbers are for describing specific embodiments and do not constitute a limitation on the scope of protection of the present invention.

[0022] Unless otherwise specified, the experimental methods used in the present invention are all conventional methods, and the materials, reagents, etc. used are all commercially available unless otherwise specified.

[0023] Unless otherwise specified, % and percentages are by mass.

[0024] In the present invention:

[0025] Australian blue cypress wood oil refers to Australian blue cypress (CALLITRIS INTRATROPICA) wood oil.

[0026] Juniper oil refers to North American juniper (JUNIPERUS VIRGINIANA) oil.

[0027] Sage oil refers to sage oil (SALVIA OFFICINALIS).

[0028] Lavender sage oil refers to lavender sage (SALVIA LAVANDULIFOLIA) leaf oil.

[0029] Gum arabic refers to the gum of the gum arabic tree (ACACIA SENEGAL).

[0030] Example 1 Preparation of an oil-controlling and acne-removing composition, comprising the following steps:

[0031] S1 Weighing of raw materials: Weigh the raw materials according to the following mass parts:

[0032]

[0033] S2 core material pre-emulsification: salicylic acid is mixed with Australian blue cedar oil and sage oil and dissolved in ethanol; the amount of ethanol used is twice that of the solute; sodium dihydrogen phosphate is then added to adjust the pH to 5.0, and shear emulsification is performed to form a core material emulsion; the shear emulsification temperature is controlled at 40-60°C and the time is 30 minutes.

[0034] S3 wall material solution preparation: dissolve hydroxypropyl cyclodextrin, cyclodextrin, and gum arabic in water; then add sodium hydroxide to adjust the solution pH to 8.0. The wall material solution preparation temperature is 60-80°C to form a wall material solution with a solid content of 30%;

[0035] S4 microencapsulation: the core material emulsion and the wall material solution are mixed and then homogenized into a uniform emulsion; a freeze-drying method is used to obtain an oil-controlling and anti-acne composition encapsulating salicylic acid.

[0036] Example 2 Preparation of an oil-controlling and acne-removing composition, comprising the following steps:

[0037] S1 Weighing of raw materials: Weigh the raw materials according to the following mass parts:

[0038]

[0039] S2 core material pre-emulsification: salicylic acid is mixed with Australian blue cedar oil and medicinal sage oil and dissolved in ethanol; the amount of ethanol used is twice that of the solute; sodium dihydrogen phosphate is then added to adjust the pH to 6.5, and shear emulsification is performed to form a core material emulsion; the shear emulsification temperature is controlled at 40-60°C and the time is 30 minutes.

[0040] S3 wall material solution preparation: dissolve hydroxypropyl cyclodextrin, cyclodextrin, and gum arabic in water; then add sodium hydroxide to adjust the solution pH to 8.5. The wall material solution preparation temperature is 60-80°C to form a wall material solution with a solid content of 35%;

[0041] S4 microencapsulation: the core material emulsion and the wall material solution are mixed and then homogenized into a uniform emulsion; a freeze-drying method is used to obtain an oil-controlling and anti-acne composition encapsulating salicylic acid.

[0042] Example 3 Preparation of an oil-controlling and acne-removing composition, comprising the following steps:

[0043] S1 Weighing of raw materials: Weigh the raw materials according to the following mass parts:

[0044]

[0045] S2 core material pre-emulsification: salicylic acid is mixed with Australian blue cedar oil and medicinal sage oil and dissolved in ethanol; the amount of ethanol used is twice that of the solute; sodium dihydrogen phosphate is then added to adjust the pH to 6.5, and shear emulsification is performed to form a core material emulsion; the shear emulsification temperature is controlled at 40-60°C and the time is 30 minutes.

[0046] S3 wall material solution preparation: dissolve hydroxypropyl cyclodextrin, cyclodextrin, and gum arabic in water; then add sodium hydroxide to adjust the solution pH to 9.0. The wall material solution preparation temperature is 60-80°C to form a wall material solution with a solid content of 40%;

[0047] S4 microencapsulation: the core material emulsion and the wall material solution are mixed and then homogenized into a uniform emulsion; a freeze-drying method is used to obtain an oil-controlling and anti-acne composition encapsulating salicylic acid.

[0048] Example 4 Preparation of an oil-controlling and acne-removing composition, comprising the following steps:

[0049] S1 Weighing of raw materials: Weigh the raw materials according to the following mass parts:

[0050]

[0051] S2 core material pre-emulsification: salicylic acid is mixed with Australian blue cedar oil and sage oil and dissolved in ethanol; the amount of ethanol used is twice that of the solute; sodium dihydrogen phosphate is then added to adjust the pH to 5.0, and shear emulsification is performed to form a core material emulsion; the shear emulsification temperature is controlled at 40-60°C and the time is 30 minutes.

[0052] S3 wall material solution preparation: dissolve hydroxypropyl cyclodextrin in water; then add sodium hydroxide to adjust the solution pH to 8.0. The wall material solution preparation temperature is 60-80°C to form a wall material solution with a solid content of 30%;

[0053] S4 microencapsulation: the core material emulsion and the wall material solution are mixed and then homogenized into a uniform emulsion; a freeze-drying method is used to obtain an oil-controlling and anti-acne composition encapsulating salicylic acid.

[0054] Example 5 Preparation of Oil Control and Acne Removing Composition

[0055] The difference from Example 1 is that, in the raw materials weighed in step S1, 17 parts of Australian blue cedar oil are used, and no sage oil is added.

[0056] Example 6 Preparation of Oil Control and Acne Removing Composition

[0057] The difference from Example 1 is that, in the weighing of raw materials in step S1, 17 parts of sage oil are used, and no Australian blue cedar oil is added.

[0058] Example 7 Preparation of Oil Control and Acne Removal Composition

[0059] The difference from Example 1 is that, in the raw materials weighed in step S1, salicylic acid is 52 parts; and Australian blue cedar oil and sage oil are not added.

[0060] Example 8 Preparation of Oil Control and Acne Removal Composition

[0061] The difference from Example 1 is that in the weighing of raw materials in step S1, an equal mass of juniper oil is used instead of Australian blue cedar oil.

[0062] Example 9 Preparation of Oil Control and Acne Removing Composition

[0063] The difference from Example 1 is that, in the weighing of raw materials in step S1, lavender leaf sage oil of equal mass is used instead of sage oil.

[0064] Performance Testing

[0065] (1) Allergy test

[0066] The four components of Examples 1-4 were dissolved in water to prepare a test sample with a concentration of 5%; and a human skin patch test was performed according to the "2022 Cosmetic Safety Technical Specifications";

[0067] The method of skin occlusion patch test is: select 30 people aged 18-60 years old, and select an area not exceeding 50mm 2, a qualified patch test device with a depth of approximately 1mm. Place 0.020mL of the prepared product into the patch test chamber. The control well serves as a blank control (no substance). Apply the patch test chamber containing the finished product to the subject's flexed forearm using hypoallergenic tape. Apply gentle pressure with the palm of your hand to evenly adhere the patch to the skin for 24 hours. Observe the skin for standard reactions 30 minutes after removal of the finished product (after the indentation disappears), 24 hours, and 48 hours afterward, and record the results. Each subject undergoes measurements in five sets of product and control wells.

[0068] The reaction level of all subjects was "-", level 0 reaction; that is, negative reaction, no allergic reaction occurred.

[0069] (2) Safety testing

[0070] According to the sanitary chemical inspection method section and the microbiological inspection method section in the "Technical Specifications for Safety of Cosmetics 2022 Edition" (Draft for Comments), the samples of all embodiments were tested for mercury, lead, arsenic, cadmium, total mold and yeast counts, heat-resistant coliform group, Pseudomonas aeruginosa group, and Staphylococcus aureus, and all met the corresponding indicator standard requirements.

[0071] (3) Oil control performance test

[0072] Surface skin oil content was determined using the method from the industry association guideline T / ZHCA002-2018 Test Method for Oil Control Efficacy of Cosmetics.

[0073] The sample is derived from the finished product of the above embodiment and dissolved in water to prepare a test sample with a concentration of 2%.

[0074] The testers are valid subjects who meet the voluntary inclusion and exclusion criteria.

[0075] After using the test product for two hours, the difference in oil content between the test area and the control area was recorded. The results are shown in Table 1 below.

[0076] Table 1 Difference structure of oil content between test parts and control parts (mean ± standard deviation)

[0077]

[0078] As can be seen from the data in Table 1, Example 4's wall material does not use cyclodextrin and gum arabic, relying solely on hydroxypropyl cyclodextrin, which may reduce the sustained release efficiency of the active ingredient and slightly weaken the oil control effect. Example 7 contains only salicylic acid as the ingredient, and its oil control effect is better.

[0079] Examples 5 and 6 used a single essential oil component; 8 and 9 respectively used closely related plant essential oils to replace the components specified in the present invention, which resulted in a slight decrease in their oil control effects, reflecting that the Australian blue cypress oil and sage oil of the present invention have a good synergistic effect.

[0080] (4) Acne removal performance test

[0081] The anti-acne performance of the present invention was tested using the antibacterial rate test of Propionibacterium acnes

[0082] Test method:

[0083] 1 Experimental materials and methods

[0084] Instruments and equipment: anaerobic incubator, vertical high-pressure steam sterilizer, reagents, phosphate buffer, reinforced Clostridium culture medium (RCM), Propionibacterium acnes.

[0085] 2 Experimental methods

[0086] 2.1 Sample processing

[0087] Sample: Dilute with sterile water to a sample concentration of 2%;

[0088] Blank control: phosphate buffer;

[0089] Control sample group: Propionibacterium acnes suspension + phosphate buffer.

[0090] 2.2 Test steps

[0091] Take a suspension of Propionibacterium acnes and add it to each test sample and control sample, mix thoroughly, and start timing. When the designated exposure time has elapsed, dilute the suspension appropriately. Take two to three dilutions and place the test sample and control sample onto two separate plates. Pour reinforced Clostridium difficile medium (RCM) over the suspension and mix thoroughly. Once the suspension solidifies, flip the plates over and incubate in an anaerobic incubator for 48 hours. Count the viable bacteria.

[0092] 3 Calculation formula

[0093] Inhibition rate = (AB) / A × 100%;

[0094] Where: A-average colony count of control samples; B-average colony count of test samples.

[0095] 4 Data Analysis

[0096] Evaluation criteria: If the antibacterial rate is ≥50%-90%, the product has antibacterial effect; if the antibacterial rate is ≥90%, the product has a strong antibacterial effect.

[0097] 5 Test results

[0098] The oil-controlling and anti-acne compositions of Examples 1-9 were tested according to the above method. The results are shown in Table 2.

[0099] Table 2 Antibacterial rate test results of 2% concentration samples

[0100]

[0101] In Table 2, the inhibition time is 10 min.

[0102] As shown in Table 2, Example 4's wall material, which relies solely on hydroxypropyl cyclodextrin and neither cyclodextrin nor gum arabic, has little impact on the antibacterial effect. Example 7, which contains only salicylic acid and lacks essential oils, significantly reduces its antibacterial effect against P. acnes.

[0103] Examples 5 and 6 used a single essential oil component; 8 and 9 respectively used closely related plant essential oils to replace the components specified in the present invention, which resulted in a slight decrease in their antibacterial effects, reflecting that the Australian blue cypress oil and sage oil of the present invention have a good synergistic effect.

[0104] In summary, from the experimental data in Tables 1 and 2, salicylic acid has the most significant effect on oil control; while Australian blue cypress oil and sage oil have a greater impact on acne removal; however, when Australian blue cypress oil and sage oil are used to replace part of the salicylic acid dosage, the change in oil control effect is small; but the oil control effect can be greatly improved; and the combination of Australian blue cypress oil and sage oil has a better effect than other similar essential oils.

[0105] It should be noted that the workflow described above is merely illustrative and does not limit the scope of protection of the present invention. In practical applications, technicians in this field can select part or all of it according to actual needs to achieve the purpose of the embodiment scheme, and no limitation is made here.

[0106] In addition, for technical details not fully described in this embodiment, please refer to the parameter operation method provided in any embodiment of the present invention, and will not be repeated here.

[0107] It should be noted that, in this document, the terms "comprises," "includes," or any other variations thereof are intended to encompass non-exclusive inclusion, such that a process, method, article, or system comprising a series of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or system. In the absence of further limitations, an element defined by the phrase "comprising a ..." does not exclude the presence of other identical elements in the process, method, article, or system comprising the element.

[0108] The serial numbers of the above embodiments of the present invention are for description only and do not represent the advantages or disadvantages of the embodiments.

[0109] The above are only preferred embodiments of the present invention and are not intended to limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made using the contents of the present invention specification, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. An oil-controlling and acne-removing composition encapsulating salicylic acid, characterized in that: The following components are included in parts by mass:

2. The oil-control and acne-removing composition containing salicylic acid according to claim 1, wherein: The wrapping wall material includes at least one of the following components: Hydroxypropyl cyclodextrin, cyclodextrin, gum arabic.

3. The oil-control and acne-removing composition containing salicylic acid according to claim 2, wherein: The wrapping wall material is a mixture of hydroxypropyl cyclodextrin, cyclodextrin and gum arabic, and the mass ratio thereof is 20-25:15-20:3-5.

4. The method for preparing the oil-controlling and anti-acne composition encapsulated with salicylic acid according to any one of claims 1 to 3, characterized in that: The following steps are involved: S1 Core material pre-emulsification: Salicylic acid, Australian blue cedar oil, and sage oil are mixed and dissolved in ethanol; sodium dihydrogen phosphate is then added to adjust the pH to 5.0-6.5, and shear emulsification is performed to form a core material emulsion; S2 wall material solution preparation: dissolve the wrapped wall material in water; then add sodium hydroxide to adjust the solution pH to 8.0-9.0 to form a wall material solution with a solid content of 30-40%; S3 microencapsulation: the core material emulsion and the wall material solution are mixed, and then homogenized into a uniform emulsion and dried to obtain an oil-controlling and anti-acne composition encapsulating salicylic acid.

5. The method for preparing the oil-controlling and anti-acne composition encapsulated with salicylic acid according to claim 4, characterized in that: In the step S1 of pre-emulsification of the core material, the shear emulsification temperature is ≤60° C., and the amount of ethanol used is at least twice the mass of salicylic acid.

6. The method for preparing the oil-controlling and anti-acne composition encapsulated with salicylic acid according to claim 4, characterized in that: In the preparation of the S2 wall material solution, the temperature of the wall material solution is 60-80°C.

7. Use of the oil-controlling and anti-acne composition encapsulating salicylic acid according to any one of claims 1 to 3 in the preparation of cosmetics.

8. The use according to claim 7, characterized in that The cosmetics include facial cream, essence, lotion, facial mask, toner or facial cleanser.

9. The use according to claim 7 or 8, characterized in that The mass percentage of the oil-controlling and anti-acne composition encapsulating salicylic acid in the leave-on cosmetics is at least 1%.

Images