Salicylic acid-containing moisturizing, whitening and cutin-removing essence and preparation method thereof
By mixing salicylic acid with other ingredients and wrapping it with dextrin, the problem of salicylic acid being difficult to dissolve in water and irritating the skin is solved, and efficient acne-removing and oil-controlling, whitening and antioxidant effects are achieved. And improves the moisturizing and safety of the product.
Patent Information
- Application Number
- CN202411887101.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-20
- Publication Date
- 2025-02-11
AI Technical Summary
Salicylic acid is hard to dissolve in water and can easily produce crystallization directly into skin care formulas, affecting the effect and stability, and high content of alcohol and surfactants will irritate the skin and limit its application.
Salicylic acid complex is prepared by mixing salicylic acid, silanediol salicylate, sesame amino acids and amino acid modifications and wrapping with dextrin to increase the water solubility of salicylic acid and reduce its irritability.
It improves the water solubility and skin permeability of salicylic acid, reduces irritation, and achieves the effects of acne-removing and oil control, whitening and antioxidant. The product has excellent moisturizing properties and is safe and non-irritating.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of cosmetics, and in particular to a moisturizing, whitening and keratin-removing essence containing salicylic acid and a preparation method thereof. Background Art
[0002] Salicylic acid, a white crystalline fat-soluble organic acid, is naturally present in plants such as willow bark, holly, and birch, and is a key raw material for the preparation of drugs such as aspirin. Salicylic acid has excellent effects on regulating keratin, inhibiting bacteria and inflammation, and inhibiting skin aging. It is widely used and is often used in cosmetics to play skin care roles such as acne removal, whitening, shrinking pores, and oil control. However, salicylic acid is difficult to dissolve in water, and it is easy to crystallize when directly added to the formula of skin care products, affecting its effect and stability and reducing its bioavailability. In order to ensure the stability of the product and avoid the crystallization of salicylic acid, a large amount of alcohol and surfactants are often needed in actual applications to aid solubilization. However, the high content of alcohol and surfactants in skin care products can irritate the skin, resulting in limitations in the use of salicylic acid.
[0003] In order to reduce the application limitations of salicylic acid, chemical modification, liposomalization, microencapsulation, supramolecularization and other methods are often used in practical applications to improve the solubility and irritation problems of salicylic acid.
[0004] CN115607468A discloses a supermolecular salicylic acid composition, a preparation method and its application, wherein the supermolecular salicylic acid composition is composed of the following weight proportions: 5-60 parts of salicylic acid, 5-50 parts of amino acids, 1-30 parts of polysaccharides, and 1-40 parts of cyclodextrin. The invention uses cyclodextrin to encapsulate the salicylic acid supermolecule, and utilizes the cyclic cavity molecular characteristics of the cyclodextrin molecule. The main molecule has a large cavity structure, which is sufficient to accommodate the guest molecule-supermolecular salicylic acid to form a molecular capsule. Through this molecular encapsulation, the supermolecular salicylic acid has better water-soluble dispersibility, and the resulting very low irritation, higher bioavailability and other advantages. The composition of the invention has good water solubility and low irritation, especially in line with the later application of cosmetics and personal washing products, and has the advantages of high bioavailability and the difficulty of precipitation of salicylic acid in the later product crystallization. However, the invention does not have obvious effects on enhancing the efficacy of salicylic acid in combating acne, excessive oil secretion and other problems.
[0005] CN105106108A discloses a supramolecular controlled-release salicylic acid formula and its preparation technology, which mixes salicylic acid alcohol solution, starch nanocrystal poloxamer suspension, α-cyclodextrin aqueous solution, low molecular weight fish collagen aqueous solution, and trehalose aqueous solution, and obtains a novel supramolecular controlled-release salicylic acid after ultrasonic treatment. The novel controlled-release supramolecular salicylic acid gel of the invention is composed of several active ingredients, and each ingredient has a synergistic effect, which not only effectively exerts the effect of salicylic acid on acne, but also has unexpected controlled-release effect, high transdermal efficiency, stable dosage form, heat resistance, low incidence of adverse reactions and other advantages. However, its preparation process has the disadvantages of complex process, many ingredients, sticky skin feel, unclear use effect, and irritation. Summary of the invention
[0006] In view of the above-mentioned defects of the prior art, the present invention provides a moisturizing, whitening and keratin removal essence containing salicylic acid, which has excellent acne removal, oil control, freckle lightening and whitening effects, has excellent antioxidant and keratin removal effects, and has excellent moisturizing properties. It is safe and non-irritating, can quickly and efficiently achieve the effects of acne removal and oil control, and is beneficial to skin recovery.
[0007] To achieve the above object, the present invention provides a method for preparing a moisturizing, whitening and keratin removing essence containing salicylic acid, comprising the following steps:
[0008] (1) Mix skin conditioning agent I and water, raise the temperature to 80-85°C, and stir to obtain phase A;
[0009] (2) Mix moisturizer I, surfactant I, moisturizer II, moisturizer III, surfactant II, skin conditioner II, and skin conditioner III, raise the temperature to 80-85° C., and stir to obtain phase B;
[0010] (3) Add phase A to phase B and stir until homogeneous; cool to 40-45°C and stir until uniform to obtain a liquid;
[0011] (4) sending the liquid obtained in step (3) for quality inspection, and discharging the liquid after passing the quality inspection;
[0012] (5) Filling to obtain the finished essence.
[0013] Preferably, the mass percentage of each component is:
[0014] Skin conditioner I 0.5-2%, moisturizer I 2-5%, surfactant I 0.05-0.08%, moisturizer II 0.05-1%, moisturizer III 0.2-1%, surfactant II 0.3-0.5%, skin conditioner II 0.05-0.015%, skin conditioner III 0.05-0.015%, and the balance is water.
[0015] Preferably, the humectant I is glycerin.
[0016] Preferably, the surfactant I is prepared by mixing poloxamer 407 and butylated hydroxytoluene in a mass ratio of 1:1.
[0017] Preferably, the moisturizing agent II is polyethylene glycol-8.
[0018] Preferably, the moisturizing agent III is propylene glycol.
[0019] Preferably, the surfactant II is laureth-4.
[0020] Preferably, the skin conditioning agent II is dipotassium glycyrrhizinate.
[0021] Preferably, the skin conditioning agent III is bisabolol.
[0022] Preferably, the preparation method of the skin conditioning agent I comprises the following steps, measured by weight:
[0023] Mix 1.5-3.5 parts of methylpropanediol, 1.5-3.5 parts of dipropylene glycol, 1-2 parts of PEG / PPG-14 / 7 dimethyl ether, 2.5-3.5 parts of poloxamer 407 and 1-2 parts of water, then add 7-10 parts of dextrin, stir at 300-600rpm and 30-60℃ for 5-10min, add 65-75 parts of salicylic acid, 5-15 parts of silanediol salicylate, 0.02-0.05 parts of sesame amino acids and 0-0.5 parts of amino acid modifier while stirring, then stir at 300-600rpm and 40-70℃ for 1-3h; then filter, collect the precipitate, and dry the precipitate to obtain a salicylic acid complex, i.e., skin conditioner I.
[0024] Further preferably, the preparation method of the skin conditioning agent I can also be, by weight:
[0025] Mix 1.5-3.5 parts of methyl propanediol, 1.5-3.5 parts of dipropylene glycol, 1-2 parts of PEG / PPG-14 / 7 dimethyl ether, 2.5-3.5 parts of poloxamer 407 and 1-2 parts of water, then add 7-10 parts of dextrin, stir at 300-600 rpm and 30-60°C for 5-10 minutes, add 65-75 parts of salicylic acid, 5-15 parts of silanediol salicylate, 0.02-0.05 parts of sesame amino acids while stirring. and 0-0.5 parts of amino acid modifier, and then stirred at 300-600rpm, 40-70℃ for 1-3h; then filtered, collected the precipitate, and dried the precipitate to obtain a salicylic acid complex; then added the salicylic acid complex, functional agent, and xanthan gum in a mass ratio of 1:0.1-0.2:0.1-0.2 to 30-50 parts of water, stirred at 200-500rpm for 20-40min until the solution is evenly mixed, and then dried to obtain skin conditioner I.
[0026] Preferably, the preparation method of the amino acid modification comprises the following steps, measured by weight:
[0027] S1. Mix 7-15 parts of amino acids with 50-70 parts of n-propanol, stir at room temperature and 500-800 rpm, add 30-35 parts of trimethylsilyl chloride while stirring, then raise the temperature to 65-75° C., continue to stir for 22-25 hours, and obtain a mixed solution; dry the mixed solution through a rotary evaporator to obtain a crude product; wash the crude product with ether to obtain a pre-purified product; mix the pre-purified product with 3-5 times the weight of chloroform, stir for 20-30 minutes, and then filter to collect the filtrate; dry the filtrate through a rotary evaporator to obtain a purified product, and then vacuum dry the purified product at 55-65° C. for 22-25 hours to obtain a crude product;
[0028] S2. Mix the crude product obtained above with 1-2 times the weight of water, and then add 13-17 parts of 20-30wt% ammonia aqueous solution, mix and stir for 3-5 minutes to obtain a mixed solution; extract the mixed solution with ether of 1 / 5-1 / 3 of the volume of the mixed solution, extract three times, collect the organic layer and dry it with anhydrous sodium sulfate, and then dry it on a rotary evaporator to obtain an amino acid modified product.
[0029] More preferably, in step S1, the amino acid is selected from one of L-proline, L-leucine and glycine.
[0030] Further preferably, the preparation method of the functional agent comprises the following steps, measured by weight:
[0031] 0.08-0.15 parts of ellagic acid and 0.01-0.03 parts of urea are mixed and stirred for 3-5 minutes to obtain a mixture; the mixture is then dissolved in 40-50 parts of ethanol to obtain a mixed solution, and the mixed solution is placed at 40-45° C. and 55-60 mbar for rotary evaporation to obtain a functional agent.
[0032] The present invention also provides a moisturizing, whitening and keratin-removing essence containing salicylic acid, which is prepared by the above method.
[0033] In the present invention, glycerin is a widely used moisturizer. In the moisturizing, whitening and exfoliating essence containing salicylic acid, glycerin can help alleviate the dryness of the skin that may be caused by salicylic acid, while enhancing the solubility and absorbability of other ingredients, thereby improving the moisturizing effect of the product.
[0034] The bisabolol in the present invention is a natural ingredient present in chamomile flowers, which has anti-inflammatory and soothing effects and can reduce skin inflammation and redness. At the same time, bisabolol also has a whitening effect, can inhibit the production of melanin, reduce pigmentation, and thus brighten the skin color. In the essence, it can cooperate with salicylic acid to play a dual role of anti-inflammatory and whitening, while reducing the skin irritation that may be caused by salicylic acid.
[0035] In the present invention, dipotassium glycyrrhizinate is an ingredient extracted from licorice, and has anti-inflammatory, anti-allergic, moisturizing and other effects. It can reduce skin inflammation, soothe sensitive skin, and promote the repair of skin barrier. Dipotassium glycyrrhizinate can also inhibit the activity of tyrosinase and reduce the generation of melanin, thereby achieving a whitening effect. In a moisturizing, whitening and keratinizing essence containing salicylic acid, dipotassium glycyrrhizinate can reduce the skin irritation that may be caused by salicylic acid, improve the tolerance of the skin, and enhance the whitening and moisturizing effects.
[0036] The silanediol salicylate in the present invention is a salicylic acid derivative that can stimulate the growth of collagen and elastin fibers in the skin and increase skin density. In addition, it can improve the communication between keratinocytes and fibroblasts, activate cell functions, have a soothing and anti-allergic effect, and have a cell barrier function. In a moisturizing, whitening and keratin removal essence containing salicylic acid, silanediol salicylate can help reduce inflammation and promote skin health. At the same time, due to its antioxidant properties, it may help brighten and whiten the skin.
[0037] The sesame amino acids in the present invention are a class of amino acid derivatives with special structures and functions, which have antioxidant effects, can neutralize free radicals, protect cells from oxidative damage, and delay the skin aging process. In moisturizing, whitening and exfoliating essences, sesame amino acids may help provide antioxidant protection, enhance the skin's self-defense ability, and promote skin health and repair, thereby assisting in the effects of acne removal and oil control.
[0038] Beneficial effects of the present invention:
[0039] 1. Compared with the prior art, the present invention provides a moisturizing, whitening and keratin removal essence containing salicylic acid. The essence provided contains salicylic acid, silanediol salicylate, sesame amino acids, functional agents, glycerin, bisabolol, dipotassium glycyrrhizinate, etc. The various ingredients are compounded and used, and have good acne removal, oil control, spot lightening and whitening effects, good antioxidant and keratin removal effects, and excellent moisturizing properties. It is safe and non-irritating, can quickly and efficiently achieve the effect of acne removal and oil control, and is beneficial to skin recovery.
[0040] 2. The present invention prepares a salicylic acid complex by mixing salicylic acid, silanediol salicylate, sesame amino acids and amino acid modifiers, and then encapsulating them with dextrin, which not only increases the water solubility of salicylic acid, but also reduces the irritation caused by it. In addition, the introduction of amino acid modifiers and the coordinated use of salicylic acid may be beneficial to improving the skin penetration effect of salicylic acid, so that salicylic acid can penetrate deep into the pores, dissolve the oil and keratin in the pores, thereby reducing the blockage of pores, helping to reduce the formation of acne and the secretion of oil, while promoting the metabolism of the stratum corneum, helping to remove dead skin cells, and better exerting the whitening and keratin removal effect.
[0041] 3. The present invention mixes ellagic acid with urea, and then prepares a functional agent by solvent evaporation, which not only improves the water solubility and antioxidant properties of ellagic acid, but also helps improve the whitening, moisturizing and exfoliating effects of the essence. The introduction of salicylic acid complex and xanthan gum mixed with the functional agent further improves the water solubility, antioxidant properties and stability of ellagic acid. The reason for the analysis may be that the water solubility and antioxidant properties of ellagic acid are promoted by the interaction between ellagic acid and urea to form a complex, and xanthan gum and salicylic acid complex are mixed with the functional agent, and the water solubility of ellagic acid is further increased by interaction between the three, and its stability is improved at the same time. Xanthan gum and salicylic acid complex may increase the resistance of ellagic acid to environmental factors such as temperature fluctuations and illumination by forming a protective layer, thereby improving the stability of ellagic acid, extending the storage time, so that ellagic acid can better play its whitening, moisturizing and exfoliating effects in the moisturizing, whitening and exfoliating essence. DETAILED DESCRIPTION
[0042] Parameters for specific chemical substances used, sources.
[0043] Laureth-4, CAS No.: 68439-50-9;
[0044] Example 1
[0045] A method for preparing a moisturizing, whitening and keratin removing essence containing salicylic acid comprises the following steps:
[0046] 1. Mix 1.5 g of skin conditioner I and 93.828 g of water, heat to 82°C, and stir to obtain phase A;
[0047] 2. Mix 3.5 g glycerol, 0.07 g surfactant I, 0.08 g polyethylene glycol-8, 0.6 g propylene glycol, 0.4 g laureth-4, 0.01 g dipotassium glycyrrhizate, and 0.012 g bisabolol, raise the temperature to 82° C., and stir to obtain phase B;
[0048] 3. Add phase A to phase B and stir to homogenize; cool to 43°C and stir until uniform to obtain a liquid;
[0049] 4. Send the liquid obtained in step 3 to quality inspection, and discharge it after passing the quality inspection;
[0050] 5. Filling to obtain the finished essence.
[0051] The surfactant I is prepared by mixing poloxamer 407 and butylated hydroxytoluene in a mass ratio of 1:1.
[0052] The preparation method of the skin conditioning agent I comprises the following steps:
[0053] Mix 2.5 g of methyl propanediol, 2.5 g of dipropylene glycol, 1.25 g of PEG / PPG-14 / 7 dimethyl ether, 3.125 g of poloxamer 407 and 1.875 g of water, then add 8.1 g of dextrin, stir at 550 rpm and 45°C for 8 min, add 70.625 g of salicylic acid, 10 g of silanediol salicylate, and 0.025 g of sesame amino acids while stirring, then stir at 550 rpm and 55°C for 2 h; then filter, collect the precipitate, and dry the precipitate to obtain a salicylic acid complex, i.e., skin conditioner I.
[0054] Example 2
[0055] A method for preparing a moisturizing, whitening and keratin removing essence containing salicylic acid comprises the following steps:
[0056] 1. Mix 1.5 g of skin conditioner I and 93.828 g of water, heat to 82°C, and stir to obtain phase A;
[0057] 2. Mix 3.5 g glycerol, 0.07 g surfactant I, 0.08 g polyethylene glycol-8, 0.6 g propylene glycol, 0.4 g laureth-4, 0.01 g dipotassium glycyrrhizate, and 0.012 g bisabolol, raise the temperature to 82° C., and stir to obtain phase B;
[0058] 3. Add phase A to phase B and stir to homogenize; cool to 43°C and stir until uniform to obtain a liquid;
[0059] 4. Send the liquid obtained in step 3 to quality inspection, and discharge it after passing the quality inspection;
[0060] 5. Filling to obtain the finished essence.
[0061] The surfactant I is prepared by mixing poloxamer 407 and butylated hydroxytoluene in a mass ratio of 1:1.
[0062] The preparation method of the skin conditioning agent I comprises the following steps:
[0063] Mix 2.5 g of methyl propanediol, 2.5 g of dipropylene glycol, 1.25 g of PEG / PPG-14 / 7 dimethyl ether, 3.125 g of poloxamer 407 and 1.575 g of water, then add 8.1 g of dextrin, stir at 550 rpm and 45°C for 8 min, add 70.625 g of salicylic acid, 10 g of silanediol salicylate, 0.025 g of sesame amino acids and 0.3 g of amino acid modifier while stirring, then stir at 550 rpm and 55°C for 2 h; then filter, collect the precipitate, and dry the precipitate to obtain a salicylic acid complex, i.e., skin conditioner I.
[0064] The preparation method of the amino acid modification comprises the following steps:
[0065] S1. Mix 10 g of glycine with 60 g of n-propanol, stir at room temperature and 700 rpm, add 33 g of trimethylsilyl chloride while stirring, then raise the temperature to 70°C, continue stirring for 24 hours to obtain a mixed solution; dry the mixed solution through a rotary evaporator to obtain a crude product; wash the crude product with ether to obtain a pre-purified product; mix the pre-purified product with 4 times the weight of chloroform, stir for 25 minutes, then filter and collect the filtrate; dry the filtrate through a rotary evaporator to obtain a purified product, and then vacuum dry the purified product at 60°C for 24 hours to obtain a crude product;
[0066] S2. The crude product obtained above was mixed with 1.5 times the weight of water, and then 15 g of 25 wt% aqueous ammonia solution was added, and the mixture was mixed and stirred for 4 min to obtain a mixed solution; the mixed solution was extracted with ether of 1 / 4 the volume of the mixed solution, and the extraction was performed three times. The organic layer was collected and dried with anhydrous sodium sulfate, and then dried on a rotary evaporator to obtain an amino acid modified product.
[0067] Example 3
[0068] A method for preparing a moisturizing, whitening and keratin-removing essence containing salicylic acid, which is different from Example 2 in that the method for preparing the skin conditioning agent I comprises the following steps:
[0069] Mix 2.5 g of methyl propanediol, 2.5 g of dipropylene glycol, 1.25 g of PEG / PPG-14 / 7 dimethyl ether, 3.125 g of poloxamer 407 and 1.575 g of water, then add 8.1 g of dextrin, stir at 550 rpm and 45°C for 8 min, add 70.625 g of salicylic acid, 10 g of silanediol salicylate, 0.025 g of sesame amino acids and 0.3 g of amino acid modifier while stirring, then stir at 550 rpm and 55°C for 2 h; then filter, collect the precipitate, and dry the precipitate to obtain a salicylic acid complex, i.e., skin conditioner I.
[0070] The preparation method of the amino acid modification comprises the following steps:
[0071] S1. Mix 10 g of L-leucine with 60 g of n-propanol, stir at room temperature and 700 rpm, add 33 g of trimethylsilyl chloride while stirring, then raise the temperature to 70° C., continue stirring for 24 hours to obtain a mixed solution; dry the mixed solution through a rotary evaporator to obtain a crude product; wash the crude product with ether to obtain a pre-purified product; mix the pre-purified product with 4 times the weight of chloroform, stir for 25 minutes, then filter and collect the filtrate; dry the filtrate through a rotary evaporator to obtain a purified product, and then vacuum dry the purified product at 60° C. for 24 hours to obtain a crude product;
[0072] S2. The crude product obtained above was mixed with 1.5 times the weight of water, and then 15 g of 25 wt% aqueous ammonia solution was added, and the mixture was mixed and stirred for 4 min to obtain a mixed solution; the mixed solution was extracted with ether of 1 / 4 the volume of the mixed solution, and the extraction was performed three times. The organic layer was collected and dried with anhydrous sodium sulfate, and then dried on a rotary evaporator to obtain an amino acid modified product.
[0073] Example 4
[0074] A method for preparing a moisturizing, whitening and keratin-removing essence containing salicylic acid, which is different from Example 2 in that the method for preparing the skin conditioning agent I comprises the following steps:
[0075] Mix 2.5 g of methyl propanediol, 2.5 g of dipropylene glycol, 1.25 g of PEG / PPG-14 / 7 dimethyl ether, 3.125 g of poloxamer 407 and 1.575 g of water, then add 8.1 g of dextrin, stir at 550 rpm and 45°C for 8 min, add 70.625 g of salicylic acid, 10 g of silanediol salicylate, 0.025 g of sesame amino acids and 0.3 g of amino acid modifier while stirring, then stir at 550 rpm and 55°C for 2 h; then filter, collect the precipitate, and dry the precipitate to obtain a salicylic acid complex, i.e., skin conditioner I.
[0076] The preparation method of the amino acid modification comprises the following steps:
[0077] S1. Mix 10 g of L-proline with 60 g of n-propanol, stir at room temperature and 700 rpm, add 33 g of trimethylsilyl chloride while stirring, then raise the temperature to 70° C., continue stirring for 24 hours to obtain a mixed solution; dry the mixed solution through a rotary evaporator to obtain a crude product; wash the crude product with ether to obtain a pre-purified product; mix the pre-purified product with 4 times the weight of chloroform, stir for 25 minutes, then filter and collect the filtrate; dry the filtrate through a rotary evaporator to obtain a purified product, and then vacuum dry the purified product at 60° C. for 24 hours to obtain a crude product;
[0078] S2. The crude product obtained above was mixed with 1.5 times the weight of water, and then 15 g of 25 wt% aqueous ammonia solution was added, and the mixture was mixed and stirred for 4 min to obtain a mixed solution; the mixed solution was extracted with ether of 1 / 4 the volume of the mixed solution, and the extraction was performed three times. The organic layer was collected and dried with anhydrous sodium sulfate, and then dried on a rotary evaporator to obtain an amino acid modified product.
[0079] Example 5
[0080] A method for preparing a moisturizing, whitening and keratin removing essence containing salicylic acid comprises the following steps:
[0081] 1. Mix 1.5 g of skin conditioner I and 93.828 g of water, heat to 82°C, and stir to obtain phase A;
[0082] 2. Mix 3.5 g glycerol, 0.07 g surfactant I, 0.08 g polyethylene glycol-8, 0.6 g propylene glycol, 0.4 g laureth-4, 0.01 g dipotassium glycyrrhizate, and 0.012 g bisabolol, raise the temperature to 82° C., and stir to obtain phase B;
[0083] 3. Add phase A to phase B and stir to homogenize; cool to 43°C and stir until uniform to obtain a liquid;
[0084] 4. Send the liquid obtained in step 3 to quality inspection, and discharge it after passing the quality inspection;
[0085] 5. Filling to obtain the finished essence.
[0086] The surfactant I is prepared by mixing poloxamer 407 and butylated hydroxytoluene in a mass ratio of 1:1.
[0087] The preparation method of the skin conditioning agent I comprises the following steps:
[0088] Mix 2.5g of methyl propanediol, 2.5g of dipropylene glycol, 1.25g of PEG / PPG-14 / 7 dimethyl ether, 3.125g of poloxamer 407 and 1.875g of water, then add 8.1g of dextrin, stir at 550rpm and 45°C for 8min, add 70.625g of salicylic acid, 10g of silanediol salicylate and 0.025g of sesame amino acids while stirring, and then stir at 550rpm and 55°C for 2h; then filter, collect the precipitate, and dry the precipitate to obtain a salicylic acid complex; then add the salicylic acid complex, functional agent and xanthan gum in a mass ratio of 1:0.15:0.15 to 40g of water, stir at 400rpm for 30min until the solution is evenly mixed, and then dry to obtain skin conditioner I.
[0089] The preparation method of the functional agent comprises the following steps:
[0090] 0.1 g of ellagic acid and 0.02 g of urea were mixed and stirred for 3 minutes to obtain a mixture; the mixture was then dissolved in 45 g of ethanol to obtain a mixed solution, and the mixed solution was placed at 43° C. and 57 mbar for rotary evaporation to obtain a functional agent.
[0091] Example 6
[0092] A method for preparing a moisturizing, whitening and keratin removing essence containing salicylic acid comprises the following steps:
[0093] 1. Mix 1.5 g of skin conditioner I and 93.828 g of water, heat to 82°C, and stir to obtain phase A;
[0094] 2. Mix 3.5 g glycerol, 0.07 g surfactant I, 0.08 g polyethylene glycol-8, 0.6 g propylene glycol, 0.4 g laureth-4, 0.01 g dipotassium glycyrrhizate, and 0.012 g bisabolol, raise the temperature to 82° C., and stir to obtain phase B;
[0095] 3. Add phase A to phase B and stir to homogenize; cool to 43°C and stir until uniform to obtain a liquid;
[0096] 4. Send the liquid obtained in step 3 to quality inspection, and discharge it after passing the quality inspection;
[0097] 5. Filling to obtain the finished essence.
[0098] The surfactant I is prepared by mixing poloxamer 407 and butylated hydroxytoluene in a mass ratio of 1:1.
[0099] The preparation method of the skin conditioning agent I comprises the following steps:
[0100] Mix 2.5g of methyl propanediol, 2.5g of dipropylene glycol, 1.25g of PEG / PPG-14 / 7 dimethyl ether, 3.125g of poloxamer 407 and 1.575g of water, then add 8.1g of dextrin, stir at 550rpm and 45°C for 8min, add 70.625g of salicylic acid, 10g of silanediol salicylate, 0.025g of sesame amino acids and 0.3g of amino acid modifier while stirring, then stir at 550rpm and 55°C for 2h; then filter, collect the precipitate, and dry the precipitate to obtain a salicylic acid complex; then mix the salicylic acid complex, functional agent and xanthan gum in a mass ratio of 1:0.15:0.15, add to 40g of water, and stir at 400rpm for 30min; until the solution is mixed evenly, and then dry to obtain skin conditioner I.
[0101] The preparation method of the amino acid modification is consistent with that of Example 4.
[0102] The preparation method of the functional agent is consistent with that of Example 5.
[0103] Comparative Example 1
[0104] A method for preparing a moisturizing, whitening and keratin-removing essence containing salicylic acid, which is different from Example 1 in that the method for preparing the skin conditioning agent I comprises the following steps:
[0105] Mix 2.5 g of methyl propanediol, 2.5 g of dipropylene glycol, 1.25 g of PEG / PPG-14 / 7 dimethyl ether, 3.125 g of poloxamer 407 and 1.875 g of water, then add 8.1 g of dextrin, stir at 550 rpm and 45°C for 8 min, add 70.625 g of salicylic acid and 0.025 g of sesame amino acids while stirring, then stir at 550 rpm and 55°C for 2 h; then filter, collect the precipitate, and dry the precipitate to obtain a salicylic acid complex, i.e., skin conditioner I.
[0106] Comparative Example 2
[0107] A method for preparing a moisturizing, whitening and keratin-removing essence containing salicylic acid, which is different from Example 1 in that the method for preparing the skin conditioning agent I comprises the following steps:
[0108] Mix 2.5 g of methylpropanediol, 2.5 g of dipropylene glycol, 1.25 g of PEG / PPG-14 / 7 dimethyl ether, 3.125 g of poloxamer 407 and 1.875 g of water, then add 8.1 g of dextrin, stir at 550 rpm and 45°C for 8 min, add 70.625 g of salicylic acid and 10 g of silanediol salicylate while stirring, then stir at 550 rpm and 55°C for 2 h; then filter, collect the precipitate, and dry the precipitate to obtain a salicylic acid complex, i.e., skin conditioner I.
[0109] Comparative Example 3
[0110] A method for preparing a moisturizing, whitening and keratin-removing essence containing salicylic acid, which is different from Example 5 in that the method for preparing the skin conditioning agent I comprises the following steps:
[0111] Mix 2.5g of methyl propanediol, 2.5g of dipropylene glycol, 1.25g of PEG / PPG-14 / 7 dimethyl ether, 3.125g of poloxamer 407 and 1.875g of water, then add 8.1g of dextrin, stir at 550rpm and 45°C for 8min, add 70.625g of salicylic acid, 10g of silanediol salicylate and 0.025g of sesame amino acids while stirring, and then stir at 550rpm and 55°C for 2h; then filter, collect the precipitate, and dry the precipitate to obtain a salicylic acid complex; then add the salicylic acid complex and the functional agent into 40g of water at a mass ratio of 1:0.15, stir at 400rpm for 30min until the solution is evenly mixed, and then dry to obtain skin conditioner I.
[0112] The preparation method of the functional agent is consistent with that of Example 5.
[0113] Comparative Example 4
[0114] A method for preparing a moisturizing, whitening and keratin removing essence, which is different from Example 5 in that the method for preparing the skin conditioning agent I comprises the following steps:
[0115] 5 g of the functional agent and 5 g of xanthan gum were added to 40 g of water, stirred at 400 rpm for 30 min until the solution was evenly mixed, and then dried to obtain skin conditioner I.
[0116] The preparation method of the functional agent is consistent with that of Example 5.
[0117] Test Example 1
[0118] Safety Experiment
[0119] The essences prepared in Examples 1-6 of the present invention and Comparative Examples 1-4 were subjected to safety tests. 100 volunteers aged 15-50 were selected, half of them were male and half were female; the volunteers were randomly divided into groups of 10, half of them were male and half were female, for a total of 10 groups, to test the safety of the essences obtained in Examples 1-6 of the present invention and Comparative Examples 1-4.
[0120] The specific testing method is: apply the corresponding test sample on the inner side of the right arm of each group of volunteers, 0.5g of the sample each time, and record the skin reaction phenomena after 1 hour, 4 hours, 8 hours and 24 hours; the test results show that after 1 hour, 4 hours, 8 hours and 24 hours of application, the 100 volunteers did not show skin redness or erythema and other allergic phenomena, indicating that the product of the present invention is mild, safe and non-irritating.
[0121] Test Example 2
[0122] Acne and oil control test
[0123] Test method: 110 testers aged 15-35 years old, half of whom were male and half were female, with obvious acne and blackheads on their faces were selected and randomly divided into 11 groups, with 10 people in each group, half of whom were male and half were female, and recorded as Example 1-6 group, Comparative Example 1-4 group and control group; wherein Example 1-6 group and Comparative Example 1-4 group were respectively smeared with the moisturizing, whitening and keratin removal essence prepared by Examples 1-6 and Comparative Example 1-4 of the present invention, and applied to the face once in the morning and evening after washing the face with clean water every day, with the same amount, and used continuously for 14 days; the control group only washed the face with clean water, once in the morning and evening every day, for 14 consecutive days; no other skin care products were used during the test.
[0124] Before the test and 14 days after the test, the left, middle and right sides of the face of each group of testers were photographed using facial image analysis software VISIA and Image ProPlus, and the acne scar area was analyzed using IPP. In addition, the facial oil secretion was tested using the skin oil test probe Sebumeter SM815. The acne scar reduction rate and facial oil content reduction rate were calculated based on the test results. The calculation formulas for the acne scar reduction rate and facial oil content reduction rate are as follows:
[0125] Acne scar area reduction rate (%) = (A0-A 14 ) / A0×100%
[0126] Where A0 is the acne scar area before the test, A 14 To test the acne scar area after 14 days;
[0127] Facial oil content reduction rate (%) = (B0-B 14 ) / B0×100%
[0128] Where, B0 is the fat content of the face before the test, B 14 To test the facial oil content after 14 days;
[0129] The test results are averaged, and the specific test results are shown in Table 1 below.
[0130] Table 1 Test results of acne removal and oil control in each group
[0131]
[0132]
[0133] As shown in Table 1, compared with the control group, the moisturizing, whitening and keratinizing essences prepared by Examples 1-6 of the present invention and Comparative Examples 1-4 have better acne removal and oil control effects. By comparing Examples 1-6 and Comparative Examples 1-4, it is found that the acne scar area reduction rate and facial oil content reduction rate of Examples 2-6 are significantly higher than those of Examples 1 and Comparative Examples 1-4, among which the acne scar area reduction rate and facial oil content reduction rate of Example 6 are the highest, and the acne removal and oil control effect is the best, indicating that the introduction of the salicylic acid complex containing amino acid modifiers, functional agents and xanthan gum can significantly improve the acne removal and oil control effect of the prepared moisturizing, whitening and keratinizing essence.
[0134] Compared with Example 1, Comparative Example 1 did not add silanediol salicylate when preparing the salicylic acid complex, Comparative Example 2 did not add sesame amino acids when preparing the salicylic acid complex, and Examples 2-4 introduced amino acid modifiers when preparing the salicylic acid complex. The absence of silanediol salicylate and sesame amino acids affected the acne-removing and oil-controlling effects, resulting in a worse acne-removing and oil-controlling effect; while the introduction of amino acid modifiers was beneficial to improving the acne-removing and oil-controlling effects of the essence, and Example 4 had the best improvement effect. The reason for this may be that the mixed use of amino acid modifiers and salicylic acid is beneficial to improving the transdermal permeability of salicylic acid, allowing salicylic acid to penetrate deep into the pores, dissolving the oil and keratin in the pores, thereby reducing pore blockage and helping to reduce the formation of acne and oil secretion.
[0135] Compared with Example 1, Example 5 introduces a functional agent and a xanthan gum and salicylic acid complex to prepare a skin conditioning agent I, which is applied to the moisturizing, whitening and horny essence of the present invention to significantly improve the effect of acne removal and oil control. The reason for the analysis may be that the interaction between ellagic acid and urea forms a complex that promotes the water solubility and antioxidant properties of ellagic acid, which is beneficial to improving the effect of acne removal and oil control. Mixing the xanthan gum and salicylic acid complex with the functional agent may further increase the water solubility of ellagic acid and improve its stability, thereby improving the antioxidant, anti-inflammatory and moisturizing effects of the functional agent, which is beneficial to controlling skin oil secretion and reducing the formation of acne. At the same time, it may be because xanthan gum has good hydrophilicity, which helps the dispersion and penetration of the active ingredients of the essence on the skin surface. At the same time, xanthan gum has a certain adhesiveness, which is beneficial to increase the action time of the salicylic acid complex and the functional agent on the skin surface, stimulate epidermal cell proliferation and differentiation, accelerate the metabolic process of the stratum corneum, and promote deeper skin conditioning.
[0136] Compared with Example 5, no xanthan gum is added to the skin conditioner I of Comparative Example 3, and no salicylic acid complex is added to the skin conditioner I of Comparative Example 4. The absence of xanthan gum and salicylic acid complex affects the acne-removing and oil-controlling effects, resulting in a deterioration of the acne-removing and oil-controlling effects.
[0137] Test Example 3
[0138] Stability test
[0139] The skin conditioning agent I and ellagic acid in Examples 5-6 of the present invention and Comparative Examples 3-4 were taken as samples, recorded as Example 5-6 group, Comparative Example 3-4 group and control group; each group of samples was prepared into a sample solution with an equal volume of deionized water, and then sealed and stored at room temperature and without light for 6 months and 12 months respectively; after the storage time, each group was tested and evaluated for thermal stability and light stability;
[0140] Thermal stability evaluation: Before the test treatment, the ellagic acid content of each sample solution prepared above was measured by sampling, and then heated at 60°C for 10 hours. After the test, the absorbance of ellagic acid was measured by sampling, and the change rate (%) of the absorbance of ellagic acid was calculated according to the following calculation formula, and the thermal stability of ellagic acid under different test conditions was evaluated according to the change rate of the absorbance of ellagic acid;
[0141] Light stability evaluation: Before the test treatment, each sample solution prepared above was sampled to determine the ellagic acid content, and then placed under ultraviolet light (254nm) for 96 hours. After the test, samples were taken to determine the absorbance of ellagic acid. The change rate (%) of the absorbance of ellagic acid was calculated according to the following calculation formula, and the light stability under different test conditions was evaluated according to the change rate of the absorbance of ellagic acid;
[0142] Variation rate of absorbance of ellagic acid (%) = (A0-A) / A0×100%
[0143] Wherein, A0 is the absorbance of ellagic acid before treatment; A is the rate of change of absorbance of ellagic acid after treatment;
[0144] The specific test results are shown in Table 2 below.
[0145] Table 2 Stability test results
[0146]
[0147] As shown in Table 2, the retention concentration reduction rate of ellagic acid stored for 12 months is significantly higher than the retention concentration reduction rate of ellagic acid stored for 6 months, indicating that with the extension of storage time, the retention concentration reduction rate of ellagic acid gradually increases, and the thermal stability and light stability are significantly reduced. Compared with the control group, the retention concentration reduction rate of ellagic acid in Examples 5-6 and Comparative Examples 3-4 is significantly lower than that in the control group, and the stability is better than that in the control group; by comparing Examples 5-6 and Comparative Examples 3-4, it is found that Example 5-6 is lower than Comparative Examples 3-4, indicating that the salicylic acid complex and xanthan gum are used in coordination with the functional agent, and the xanthan gum and salicylic acid complex can improve the stability of the functional agent. The reason for the analysis may be that the interaction between ellagic acid and urea forms a complex that promotes the water solubility and antioxidant properties of ellagic acid, which is beneficial to improve its stability; the xanthan gum and salicylic acid complex are mixed with the functional agent, and the interaction between the three further increases the water solubility of ellagic acid and improves its stability. Salicylic acid complex and xanthan gum may increase the resistance of ellagic acid to environmental factors such as temperature fluctuations and light by forming a wrapped protective layer on the surface of the functional agent, thereby improving its stability and reducing the risk of degradation of ellagic acid that may occur during the production and storage of cosmetics.
Claims
1. A method for preparing a moisturizing, whitening and keratin removing essence containing salicylic acid, characterized in that: The following steps are involved: (1) Mix skin conditioning agent I and water, raise the temperature to 80-85°C, and stir to obtain phase A; (2) Mix moisturizer I, surfactant I, moisturizer II, moisturizer III, surfactant II, skin conditioner II, and skin conditioner III, raise the temperature to 80-85° C., and stir to obtain phase B; (3) Add phase A to phase B and stir until homogeneous; cool to 40-45°C and stir until uniform to obtain a liquid; (4) sending the liquid obtained in step (3) for quality inspection, and discharging the liquid after passing the quality inspection; (5) Filling to obtain the finished essence.
2. The method for preparing the moisturizing, whitening and keratin removing essence containing salicylic acid as claimed in claim 1, characterized in that: The mass percentage of each component is: Skin conditioner I 0.5-2%, moisturizer I 2-5%, surfactant I 0.05-0.08%, moisturizer II 0.05-1%, moisturizer III 0.2-1%, surfactant II 0.3-0.5%, skin conditioner II 0.05-0.015%, skin conditioner III 0.05-0.015%, and the balance is water.
3. The method for preparing the moisturizing, whitening and keratin removing essence containing salicylic acid as claimed in claim 1 or 2, characterized in that: The moisturizing agent I is glycerin; the surfactant I is a mixture of poloxamer 407 and butylated hydroxytoluene in a mass ratio of 1:1; the moisturizing agent II is polyethylene glycol-8; the moisturizing agent III is propylene glycol; the surfactant II is laureth-4; the skin conditioning agent II is dipotassium glycyrrhizinate; and the skin conditioning agent III is bisabolol.
4. The method for preparing the moisturizing, whitening and keratin removing essence containing salicylic acid as claimed in claim 1 or 2, characterized in that: The preparation method of the skin conditioning agent I comprises the following steps, calculated by weight: Mix 1.5-3.5 parts of methylpropanediol, 1.5-3.5 parts of dipropylene glycol, 1-2 parts of PEG / PPG-14 / 7 dimethyl ether, 2.5-3.5 parts of poloxamer 407 and 1-2 parts of water, then add 7-10 parts of dextrin, stir at 300-600rpm and 30-60℃ for 5-10min, add 65-75 parts of salicylic acid, 5-15 parts of silanediol salicylate, 0.02-0.05 parts of sesame amino acids and 0-0.5 parts of amino acid modifier while stirring, then stir at 300-600rpm and 40-70℃ for 1-3h; then filter, collect the precipitate, and dry the precipitate to obtain a salicylic acid complex, i.e., skin conditioner I.
5. The method for preparing the moisturizing, whitening and keratin removing essence containing salicylic acid as claimed in claim 4, characterized in that: The preparation method of the skin conditioning agent I can also be, by weight: Mix 1.5-3.5 parts of methyl propanediol, 1.5-3.5 parts of dipropylene glycol, 1-2 parts of PEG / PPG-14 / 7 dimethyl ether, 2.5-3.5 parts of poloxamer 407 and 1-2 parts of water, then add 7-10 parts of dextrin, stir at 300-600 rpm and 30-60°C for 5-10 minutes, add 65-75 parts of salicylic acid, 5-15 parts of silanediol salicylate, 0.02-0.05 parts of sesame amino acids while stirring. and 0-0.5 parts of amino acid modifier, and then stirred at 300-600rpm, 40-70℃ for 1-3h; then filtered, collected the precipitate, and dried the precipitate to obtain a salicylic acid complex; then added the salicylic acid complex, functional agent, and xanthan gum in a mass ratio of 1:0.1-0.2:0.1-0.2 to 30-50 parts of water, stirred at 200-500rpm for 20-40min until the solution is evenly mixed, and then dried to obtain skin conditioner I.
6. The method for preparing the moisturizing, whitening and keratin removing essence containing salicylic acid according to claim 4 or 5, characterized in that: The preparation method of the amino acid modification comprises the following steps, calculated by weight: S1. Mix 7-15 parts of amino acids with 50-70 parts of n-propanol, stir at room temperature and 500-800 rpm, add 30-35 parts of trimethylsilyl chloride while stirring, then raise the temperature to 65-75° C., continue to stir for 22-25 hours to obtain a mixed solution; dry the mixed solution by rotary evaporator to obtain a crude product; wash the crude product with ether to obtain a pre-purified product; The pre-purified product was mixed with 3-5 times the weight of chloroform, stirred for 20-30 minutes, and then filtered to collect the filtrate; the filtrate was dried by rotary evaporator to obtain a purified product, and then the purified product was vacuum dried at 55-65° C. for 22-25 hours to obtain a crude product; S2. Mix the crude product obtained above with 1-2 times the weight of water, and then add 13-17 parts of 20-30wt% ammonia aqueous solution, mix and stir for 3-5 minutes to obtain a mixed solution; extract the mixed solution with ether of 1 / 5-1 / 3 of the volume of the mixed solution, extract three times, collect the organic layer and dry it with anhydrous sodium sulfate, and then dry it on a rotary evaporator to obtain an amino acid modified product.
7. The method for preparing the moisturizing, whitening and keratin removing essence containing salicylic acid according to claim 6, characterized in that: In step S1, the amino acid is selected from one of L-proline, L-leucine and glycine.
8. The method for preparing the moisturizing, whitening and keratin removing essence containing salicylic acid as claimed in claim 5, characterized in that: The preparation method of the functional agent comprises the following steps, measured by weight: 0.08-0.15 parts of ellagic acid and 0.01-0.03 parts of urea are mixed and stirred for 3-5 minutes to obtain a mixture; the mixture is then dissolved in 40-50 parts of ethanol to obtain a mixed solution, and the mixed solution is placed at 40-45° C. and 55-60 mbar for rotary evaporation to obtain a functional agent.
9. A moisturizing, whitening and keratin removing essence containing salicylic acid, characterized in that: Prepared by the method described in any one of 1-8.
Citation Information
Patent Citations
Supermolecule controlled / slow-release type salicylate formula and preparation technology thereof
CN105106108A
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