A high-content water-soluble idebenone suspension inclusion and preparation method thereof

Abstract

The present application relates to the field of cosmetic raw materials, and more specifically, it relates to a high-content water-soluble idebenone suspension inclusion and a preparation method thereof. A high-content water-soluble idebenone suspension inclusion comprises: 5-10% idebenone, 1-3% emulsifier, 5-15% solubilizer, 0.01-1% preservative, 15-25% alcohol solvent, and the solvent is supplemented with the remainder; its preparation method is: step 1: mixing the alcohol solvent and the solubilizer to obtain solution A; step 2: mixing idebenone with solution A to obtain solution B; step 3: mixing solution B with the solvent, heating and boiling, and ultrasonically treating for 15-30 minutes under the condition of ultrasonic power of 1200-1400W to obtain solution C; step 4: adding preservative to solution C to obtain a finished product. The present application enables idebenone to have a good mixing effect in water-based products such as lotions and maintain long-term stability.

Description

Technical Field

[0001] The present application relates to the field of cosmetic raw materials, and more specifically, to a high-content water-soluble idebenone suspension inclusion and a preparation method thereof. Background Art

[0002] Idebenone, also known as idebenone or hydroxydecylubiquinone, is a lipophilic compound. It is a highly effective antioxidant that has multiple functions such as scavenging free radicals and inhibiting lipid peroxidation, and can significantly improve skin condition.

[0003] However, due to its lipophilicity and poor solubility in water, idebenone can only be added to products such as creams, and its application in water-based products such as lotions is limited, and it can only be added in small amounts to water-based products such as cosmetics. However, even if the dosage has been reduced, due to its lipophilic nature, it is still prone to problems such as instability and poor effect.

[0004] For example, the technical solution disclosed in CN110339137A in the prior art provides a formula of yeast beauty essence and a preparation method thereof. The invention is prepared from the following raw materials in parts by weight: 70-85 parts of water, 1-10 parts of butylene glycol, 1-10 parts of dipropylene glycol, 1-8 parts of biosaccharide gum-1, 1-8 parts of bifida yeast fermentation product lysate, 1-5 parts of glucosamine, 1-4 parts of dendrobium extract, lactose, 1-4 parts of milk protein, 0.1-3 parts of yeast extract, 0.1-0.8 parts of A91 (caprylhydroxamic acid: propylene glycol: glycerol caprylate = 1:2:1), 0.1-0.6 parts of p-hydroxyacetophenone, 0.1-0.6 parts of 1,2-hexanediol, 0.1-0.5 parts of idebenone, 0.1-0.5 parts of xanthan gum, 0.05-0.3 parts of dipotassium glycyrrhizinate, and 0.01-0.2 parts of disodium EDTA. Due to the above analysis reasons, the content of idebenone is only 0.1-0.5 parts, which cannot play a significant effect.

[0005] Therefore, there is room for improvement. Summary of the invention

[0006] In order to make idebenone have a good mixing effect in water-based products such as lotions, the present application provides a high-content water-soluble idebenone suspension inclusion and a preparation method thereof.

[0007] In the first aspect, the present application provides a high-content water-soluble idebenone suspension inclusion, which adopts the following technical solution:

[0008] A high-content water-soluble idebenone suspension inclusion body comprises the following raw materials in terms of mass percentage: 5-10% idebenone, 1-3% emulsifier, 5-15% solubilizer, 0.01-1% preservative, 15-25% alcohol solvent, and the solvent supplements the balance;

[0009] The emulsifier is at least a mixture of one or more of lecithin and hydrogenated lecithin.

[0010] Idebenone is a fat-soluble substance with poor stability, which leads to its narrow application range (only applicable to creams) and easy discoloration when used in formulas. This application encapsulates it into a water-soluble product, expanding its market application range (applicable to lotions, creams, etc.). It is more stable and not easy to discolor in the formula, ensuring that the activity can be maximized.

[0011] The idebenone aqueous solution currently available on the market has a low idebenone content and is unstable (discoloration, precipitation). The present application prepares idebenone into idebenone inclusions to form a stable (no discoloration) product with uniform particle size. The high-content idebenone aqueous solution can also be better adapted to different types of lotion and cream formulas in formulation applications.

[0012] Moreover, when the inclusion is applied to downstream products, the water-based solution is sprayed on the face of a person, and when the person gently applies warm hands to the face, etc., the inclusion can smoothly release the inner inclusions, thereby giving full play to the efficacy of idebenone. Moreover, since the high content of idebenone forms inclusions, when the water-based solution is sprayed on the face, the person will not feel strong irritation; during the release process, it will not be released all at once, but will be released in an orderly manner, so as to reduce irritation as much as possible while ensuring that the efficacy is fully exerted.

[0013] Preferably, the mass percentage of the solubilizer is 10-15%.

[0014] By adopting the above technical scheme, when the mass percentage of idebenone is determined to be within a certain range, the dosage coordination relationship of the emulsifier and the solubilizer with idebenone is further limited, so that idebenone can be more fully and quickly encapsulated, thereby enhancing the stability of the inclusion body in aqueous products such as lotions.

[0015] Preferably, the solubilizer comprises at least one or more of dimethyl isosorbide, PPG-26-butanol polyether-26, cocoether-7, PPG-13-decyltetradecyl alcohol polyether-24, and diisopropyl sebacate.

[0016] Preferably, the solubilizer is dimethyl isosorbide, PPG-26-butanol polyether-26, cocoether-7, PPG-13-decyltetradecyl alcohol polyether-24, and diisopropyl sebacate. Calculated by the mass percentage of the high-content water-soluble idebenone suspended inclusions, the mass percentage of dimethyl isosorbide is 4-6%, the mass percentage of PPG-26-butanol polyether-26 is 0.5-2%, the mass percentage of cocoether-7 is 1-2%, the mass percentage of PPG-13-decyltetradecyl alcohol polyether-24 is 1-2%, and the mass percentage of diisopropyl sebacate is 1.2-3.8%.

[0017] By adopting the above technical solution and selecting a specific solubilizer, the solubility of idebenone can be increased, and the emulsifier allows the formed micelles to be better encapsulated, making the micelles less likely to demulsify, and idebenone can be better dispersed in the micelles, greatly improving the stability of the inclusion body.

[0018] The dielectric constant of the interior of the micelle is different from that of the surrounding solvent. According to the chemical properties of idebenone itself, it interacts with the micelle in different ways, so that the idebenone molecules are dispersed in the micelle.

[0019] Under the specific proportions of dimethyl isosorbide, PPG-26-butanol polyether-26, cocoether-7, PPG-13-decyltetradecyl alcohol polyether-24, and diisopropyl sebacate, the system forms a specific colloidal dispersion system, so that idebenone is encapsulated or adsorbed, the solubility of idebenone in the system is increased, and idebenone is stably dispersed and suspended in the colloidal system.

[0020] Preferably, the alcohol solvent is a mixture of one or more of glycerol, butanediol and pentanediol.

[0021] Preferably, the solvent is water.

[0022] Preferably, the preservative is ethylhexylglycerin.

[0023] In a second aspect, the present application provides a method for preparing a high-content water-soluble idebenone suspension inclusion, using the following technical solution:

[0024] A method for preparing a high-content water-soluble idebenone suspension inclusion comprises the following steps:

[0025] Step 1: Mix the alcohol solvent and the solubilizer until they are uniformly dissolved to obtain solution A;

[0026] Step 2: Mix idebenone and solution A until uniform, to obtain solution B;

[0027] Step 3: Mix solution B with the solvent, heat and boil, and then perform ultrasonic treatment for 15-30 minutes at an ultrasonic power of 1200-1400 W to obtain solution C;

[0028] Step 4: Add preservatives to solution C and mix until uniform to obtain the finished product.

[0029] Preferably, a method for preparing a high-content water-soluble idebenone suspension inclusion comprises the following steps:

[0030] Step 1: Mix the alcohol solvent and the solubilizer until they are uniformly dissolved to obtain solution A;

[0031] Step 2: Mix idebenone and solution A until uniform, to obtain solution B;

[0032] Step 3: Mix solution B with the solvent, heat and boil, and then perform ultrasonic treatment for 15-30 minutes at an ultrasonic power of 1200-1400 W to obtain solution C;

[0033] Step 4: Add the preservative to solution C and mix until uniform to obtain solution D;

[0034] Step 5: Continue stirring solution D for 5-10 minutes to obtain a high-content water-soluble idebenzene nano-inclusion solution.

[0035] By adopting the above technical solution, the solubilizer promotes the inclusion and adsorption of more idebenone in the colloidal solution, the emulsifier enables the micelles formed in the above colloidal solution to be better encapsulated, and combined with specific ultrasonic treatment conditions, the micelles are not easy to demulsify and are more stably dispersed, thereby improving the stability of the inclusion body.

[0036] Preferably, in step 2, idebenone and solution A are homogenized at 10000-13000 rpm for 1-3 min to obtain solution B.

[0037] By adopting the above technical solution, after a specific homogenization treatment, the solution A and idebenone have a better mixing effect, which is convenient for the subsequent solubilization of idebenone, so that the inclusions can be more stable and evenly dispersed. The prepared inclusions can be used in downstream products, and can have a longer-lasting stability effect, and are not easy to be stratified or discolored.

[0038] Preferably, in step 4, solution C is cooled to 35-45° C. before adding a preservative and mixing.

[0039] Preferably, step 1 and step 2 are carried out at 83-88°C.

[0040] Preferably, the mixing in step 4 is performed at 400-700 rpm.

[0041] In summary, this application has the following beneficial effects:

[0042] 1. The present application encapsulates idebenone by selecting specific solubilizers, emulsifiers, and specific ultrasonic means to form specific idebenone suspension inclusions. The idebenone active substance is effectively encapsulated, which greatly improves the stability of the inclusions, is not prone to discoloration and stratification, and is well applied in downstream water-based products.

[0043] 2. When the idebenone inclusions formed in the present application are applied to downstream products, the portion sprayed with the downstream products is gently treated with warm hands, and the inclusions smoothly and orderly release the inner inclusions, giving full play to the efficacy of idebenone while ensuring low irritation.

[0044] 3. This application uses a specific solubilizer and emulsifier, and ultrasonic means to cooperate with each other to further ensure the stability and dispersion effect of the idebenone inclusions. BRIEF DESCRIPTION OF THE DRAWINGS

[0045] Figure 1 The high-content water-soluble idebenzene nano inclusion solution prepared in Example 1.

[0046] Figure 2 This is the high-content water-soluble idebenone nano inclusion solution prepared in Comparative Example 6.

[0047] Figure 3 It is a side-by-side comparison diagram of the high-content water-soluble idebenone nano inclusion solution of Example 1 and Comparative Example 6.

[0048] Figure 4 This is an appearance diagram of Example 1 stored at -5°C. From left to right, they are schematic diagrams of storage at -5°C for 3 days, 9 days, and 15 days, respectively.

[0049] Figure 5 This is an appearance diagram of Example 1 stored at 45° C. From left to right, the diagrams are respectively stored at 45° C. for 3 days, 9 days, and 15 days.

[0050] Figure 6 This is an appearance diagram of Example 1 stored at room temperature 25° C. From left to right, the diagrams are respectively stored at room temperature 25° C. for 3 days, 9 days, and 15 days.

[0051] Figure 7 This is the appearance diagram of Comparative Example 6 stored at -5°C. From left to right, they are schematic diagrams of storage at -5°C for 3 days, 9 days, and 15 days, respectively.

[0052] Figure 8 This is the appearance of Comparative Example 6 stored at 45°C. From left to right, they are schematic diagrams of storage at 45°C for 3 days, 9 days, and 15 days, respectively.

[0053] Fig. 9 This is the appearance diagram of Comparative Example 6 stored at room temperature 25°C. From left to right, they are schematic diagrams of storage at room temperature 25°C for 3 days, 9 days, and 15 days, respectively.

[0054] Fig.10These are the eye photos of one of the volunteers using the sample tested in Example 1. The first and second rows correspond to the same time. The second row has been color processed to facilitate wrinkle observation. From left to right, these are the photos of the volunteer's eye skin in the initial state, 0.5h skin state, and 6.5h skin state.

[0055] Fig.11 This is a photo of one of the volunteers' eyes using the sample from Comparative Example 6. The first and second rows are photos taken at the same time. The second row has been color processed to facilitate wrinkle observation. From left to right, the photos are of the volunteer's eye skin in its initial state, 0.5h skin state, and 6.5h skin state. DETAILED DESCRIPTION

[0056] The present application is further described in detail below with reference to the accompanying drawings and embodiments.

[0057] The raw materials used in the following examples and comparative examples are all commercially available products.

[0058] Example

[0059] A high-content water-soluble idebenone suspension inclusion comprises the following raw materials in terms of mass percentage: 5-10% idebenone, 1-3% emulsifier, 5-15% solubilizer, 0.01-1% preservative, 15-25% alcohol solvent, and the solvent is used to supplement the balance.

[0060] The mass percentage of idebenone can be any amount among 5%, 6%, 7%, 8%, 9%, 10% and the like.

[0061] The emulsifier can be a mixture of one or more of lecithin, hydrogenated lecithin, phosphatidylcholine, hydrogenated phosphatidylcholine, etc.

[0062] The mass percentage of the emulsifier can be any amount including 1%, 1.5%, 2%, 2.5%, 3%, etc.

[0063] The mass percentage of the solubilizer can be any amount among 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, etc.

[0064] The solubilizer contains at least one or more of dimethyl isosorbide, PPG-26-butylene glycol polyether-26, cocoether-7, PPG-13-decyltetradecyl alcohol polyether-24, and diisopropyl sebacate.

[0065] Specifically, when the solubilizing agent is dimethyl isosorbide, PPG-26-butanol polyether-26, cocoether-7, PPG-13-decyltetradecyl alcohol polyether-24, and diisopropyl sebacate, according to the mass percentage of the high-content water-soluble idebenone suspended inclusions, the mass percentage of dimethyl isosorbide is 4-6%, the mass percentage of PPG-26-butanol polyether-26 is 0.5-2%, the mass percentage of cocoether-7 is 1-2%, the mass percentage of PPG-13-decyltetradecyl alcohol polyether-24 is 1-2%, and the mass percentage of diisopropyl sebacate is 1.2-3.8%.

[0066] More specifically, according to the mass percentage of the high-content water-soluble idebenone suspension inclusions, the mass percentage of isosorbide anhydride dimethyl ether can be any amount of 4%, 4.5%, 5%, 5.5%, 6%, etc.; the mass percentage of PPG-26-butanol polyether-26 can be any amount of 0.5%, 1%, 1.5%, 2%, etc.; the mass percentage of cocoether-7 is any amount of 1%, 1.2%, 1.5%, 1.8%, 2%, etc.; the mass percentage of PPG-13-decyltetradecanol polyether-24 is any amount of 1%, 1.2%, 1.5%, 1.8%, 2%, etc.; the mass percentage of diisopropyl sebacate is any amount of 1.2%, 1.5%, 2%, 2.5%, 3%, 3.5%, 3.8%, etc.

[0067] The preservative is ethylhexylglycerin.

[0068] The mass percentage of the preservative can be any amount including 0.01%, 0.05%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, etc.

[0069] The alcohol solvent may be a mixture of one or more of glycerol, butanediol, pentanediol, etc.

[0070] According to the mass percentage of the high-content water-soluble idebenone suspension inclusions, the mass percentage of glycerol is 15-25%, and the mass percentage of glycerol can be any amount of 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, etc.

[0071] The solvent contains at least water.

[0072] A method for preparing a high-content water-soluble idebenone suspension inclusion comprises the following steps:

[0073] Step 1: Heat the alcohol solvent and solubilizer to 83-88°C, mix until they are uniformly dissolved, and obtain solution A.

[0074] Specifically, the temperature may be raised to any temperature of 83°C, 84°C, 85°C, 86°C, 87°C, 88°C, etc.

[0075] Step 2: Add idebenone to solution A, heat to 83-88° C., and homogenize at 10000-13000 rpm for 1-3 min to obtain solution B.

[0076] Specifically, the temperature can be raised to any temperature among 83°C, 84°C, 85°C, 86°C, 87°C, 88°C, etc.; homogenization can be carried out at any rotation speed among 10000rpm, 10500rpm, 11000rpm, 11500rpm, 12000rpm, 12500rpm, 13000rpm, etc.; the homogenization time can be any duration among 1min, 1.5min, 2min, 2.5min, 3min, etc.

[0077] Step 3: Add the solvent to solution B, heat it up and boil it, then put it into an ultrasonic chamber, and perform ultrasonic treatment for 15-30 minutes at an ultrasonic power of 1200-1400 W to obtain solution C.

[0078] Specifically, the ultrasonic power can be any power of 1200W, 1250W, 1300W, 1350W, 1400W, etc.; the ultrasonic treatment time can be any duration of 15min, 18min, 20min, 22min, 25min, 27min, 30min, etc.

[0079] Step 4: Take solution C out of the ultrasonic chamber, add preservatives to solution C when the temperature drops to 35-45°C, and stir and mix at 400-700 rpm until uniform, to obtain solution D.

[0080] Specifically, the temperature can be cooled to any temperature among 35°C, 36°C, 37°C, 38°C, 39°C, 40°C, 41°C, 42°C, 43°C, 44°C, 45°C, etc.; the stirring condition can be any rotation speed among 400rpm, 500rpm, 600rpm, 700rpm, etc.

[0081] Step 5: Solution D is stirred for 5-10 min at 400-700 rpm to obtain a high-content water-soluble idebenzene nano-inclusion solution.

[0082] Specifically, the stirring condition can be any rotation speed of 400rpm, 500rpm, 600rpm, 700rpm, etc.; the stirring time can be any duration of 5min, 6min, 7min, 8min, 9min, 10min, etc.

[0083] Example 1

[0084] A high-content water-soluble idebenone suspension inclusion body comprises the following raw materials: idebenone, an emulsifier, a solubilizer, a preservative, an alcohol solvent and a solvent.

[0085] The emulsifier is hydrogenated lecithin; the solubilizer is dimethyl isosorbide, PPG-26-butanol polyether-26, cocoether-7, PPG-13-decyltetradecyl alcohol polyether-24, and diisopropyl sebacate; the preservative is ethylhexylglycerin; the alcohol solvent is glycerin; and the solvent is water.

[0086] The specific amount of each raw material is shown in Table 1.

[0087] The present application also discloses a method for preparing a high-content water-soluble idebenone suspension inclusion, comprising the following steps:

[0088] Step 1: Heat the alcohol solvent and the solubilizer to 85°C and mix until they are uniformly dissolved to obtain solution A.

[0089] Step 2: Add idebenone to solution A, heat to 85° C., and homogenize at 12,000 rpm for 2 min to obtain solution B.

[0090] Step 3: Add the solvent to solution B, heat it up and boil it, then put it into an ultrasonic chamber and perform ultrasonic treatment for 20 minutes at an ultrasonic power of 1300 W to obtain solution C.

[0091] Step 4: Take solution C out of the ultrasonic chamber, add preservatives to solution C when the temperature drops to 40°C, and stir and mix at 600 rpm until uniform, to obtain solution D.

[0092] Step 5: Solution D was stirred for 8 min at 600 rpm to obtain a high-content water-soluble idebenzene nano-inclusion solution.

[0093] High content of water-soluble idebenone nano inclusion solution can be referred to Figure 1 .

[0094] Example 2

[0095] A high-content water-soluble idebenone suspension inclusion body, which is different from Example 1 in that isosorbide anhydride dimethyl ether is 40 g, PPG-26-butanol polyether-26 is 5 g, cocoether-7 is 10 g, PPG-13-decyltetradecyl alcohol polyether-24 is 10 g, and diisopropyl sebacate is 38 g.

[0096] The specific dosage is shown in Table 1.

[0097] A method for preparing a high-content water-soluble idebenone suspension inclusion body, which is different from that of Example 1 in that, in step 3, ultrasonic treatment is performed for 30 minutes at an ultrasonic power of 1200 W.

[0098] Example 3

[0099] A high-content water-soluble idebenone suspension inclusion, which is different from Example 1 in that:

[0100] The amount of dimethyl isosorbide is 60 g, the amount of PPG-26-butanol polyether-26 is 20 g, the amount of cocoether-7 is 20 g, the amount of PPG-13-decyltetradecyl alcohol polyether-24 is 20 g, and the amount of diisopropyl sebacate is 12 g.

[0101] The specific dosage is shown in Table 1.

[0102] A method for preparing a high-content water-soluble idebenone suspension inclusion body is different from that of Example 1 in that, in step 3, ultrasonic treatment is performed for 15 minutes at an ultrasonic power of 1400 W.

[0103] Table 1

[0104]

[0105]

[0106] Example 4

[0107] A high-content water-soluble idebenone suspension inclusion body, which is different from Example 1 in that the solubilizers are PPG-26-butanol polyether-26 and cocoether-7, the PPG-26-butanol polyether-26 is 60g, and the cocoether-7 is 60g.

[0108] Example 5

[0109] A high-content water-soluble idebenone suspension inclusion body, which is different from Example 1 in that the solubilizer is PPG-26-butanol polyether-26, that is, the amount of PPG-26-butanol polyether-26 is 120 g.

[0110] Example 6

[0111] A high-content water-soluble idebenone suspension inclusion body, which is different from Example 1 in that isosorbide anhydride dimethyl ether is 10 g, PPG-26-butanol polyether-26 is 30 g, cocoether-7 is 30 g, PPG-13-decyltetradecyl alcohol polyether-24 is 5 g, and diisopropyl sebacate is 45 g.

[0112] Example 7

[0113] A method for preparing a high-content water-soluble idebenone suspension inclusion body is different from that of Example 1 in that step 2 is: idebenone and solution A are homogenized at 1000 rpm for 2 minutes to obtain solution B.

[0114] Comparative Example

[0115] Comparative Example 1

[0116] A high-content water-soluble idebenone suspension inclusion body, which is different from Example 1 in that the emulsifier is replaced by water.

[0117] Comparative Example 2

[0118] A high-content water-soluble idebenone suspension inclusion body, which is different from Example 1 in that the emulsifier is replaced by Tween-80.

[0119] Comparative Example 3

[0120] A high-content water-soluble idebenone suspension inclusion body, which is different from Example 1 in that the solubilizer is replaced by water.

[0121] Comparative Example 4

[0122] A method for preparing a high-content water-soluble idebenone suspension inclusion body, which is different from Example 1 in that step 3 is: mixing solution B with a solvent, heating and boiling, and then ultrasonically treating for 20 minutes at an ultrasonic power of 130 W to obtain solution C.

[0123] Comparative Example 5

[0124] A method for preparing a high-content water-soluble idebenone suspension inclusion body, which is different from Example 1 in that step 3 is: mixing solution B with a solvent, heating and boiling, and then ultrasonically treating for 20 minutes at an ultrasonic power of 2000 W to obtain solution C.

[0125] Comparative Example 6

[0126] A method for preparing a high-content water-soluble idebenone suspension inclusion body, which is different from Example 1 in that step 3 is: mixing solution B with a solvent, heating and boiling, placing in a high-speed stirrer, and stirring at a high speed of 10000 rpm for 20 minutes to obtain solution C.

[0127] The obtained high content of water-soluble idebenone suspension inclusions is referenced Figure 2 .

[0128] Performance testing

[0129] 1. Appearance and stability test: The high-content water-soluble idebenone suspension inclusions of Examples 1-7 and Comparative Examples 1-6 were placed in an environment of -5°C, 45°C, and room temperature 25°C for 3 days, 9 days, and 15 days, respectively, to observe whether crystals were precipitated, whether the color changed, and whether the transparency was observed. The results are recorded in Table 2.

[0130] The presence or absence of color change is based on the comparison of the color between the test sample stored under corresponding conditions and the freshly prepared product.

[0131] Table 2

[0132]

[0133]

[0134]

[0135]

[0136] According to the comparison of the test data of Examples 1-7 and Comparative Examples 1-6 in Table 2, it can be seen that the high-content water-soluble idebenone suspension inclusions of Examples 1-7 can maintain good stability under different conditions; the high-content water-soluble idebenone suspension inclusions of Comparative Examples 1-6 showed different degrees of crystallization, discoloration, opacity, etc. during storage under different conditions, and were not stable enough.

[0137] The side-by-side comparison of the high-content water-soluble idebenone suspension inclusions of Example 1 and Comparative Example 6 is shown in the figure. Figure 3 , the left side is Example 1, and the right side is Comparative Example 6. It can be seen that the product on the right is more turbid and heavy, the one on the left is more transparent and light, and the transparency of the right side is obviously not as good as that of the left side.

[0138] Example 1: Appearance of the sample stored at -5°C for 3 days, 9 days and 15 days. Figure 4 , stored at 45℃ for 3 days, 9 days, 15 days, refer to the appearance diagram Figure 5 , stored at room temperature 25℃ for 3 days, 9 days, 15 days, refer to the appearance diagram Figure 6 .

[0139] The appearance of comparative example 6 stored at -5°C for 3 days, 9 days and 15 days is shown in Fig. Figure 7 , stored at 45℃ for 3 days, 9 days, 15 days, refer to the appearance diagram Figure 8 , stored at room temperature 25℃ for 3 days, 9 days, 15 days, refer to the appearance diagram Fig. 9 .

[0140] 2. Downstream product application testing:

[0141] 1. Preparation of test samples:

[0142] According to mass percentage, the test samples include the following raw materials:

[0143] Phase A: 0.15% EDTA, 0.15% panthenol, 1% butylene glycol, 1% glycerin, 0.1% allantoin, 0.05% hyaluronic acid, 0.15% carbomer U30, 0.5% p-hydroxyacetophenone, 86.45% water;

[0144] Phase B: 0.15% arginine;

[0145] Phase C: 0.5% 1,2-hexanediol, 10% efficacy.

[0146] The functional substance is the high-content water-soluble idebenone suspension inclusions of Examples 1-7 and Comparative Examples 1-6.

[0147] The specific preparation method is: homogenize the raw materials of phase A at a speed of 12000 rpm for 2 minutes, stir and cool to 55°C, then add the raw materials of phase B and stir until uniform; then cool to 45°C and add the raw materials of phase C, stir until uniform, and cool to room temperature to obtain the test sample (skin care water).

[0148] 2. Appearance and stability testing:

[0149] The test samples corresponding to Examples 1-7 and Comparative Examples 1-6 were placed in an environment of -5°C, 45°C, and room temperature 25°C for 30 days respectively, and observed for stratification, crystal precipitation, color change, and transparency. The results are recorded in Table 3.

[0150] The presence or absence of color change is based on the comparison of the color between the test sample stored under corresponding conditions and the freshly prepared product.

[0151] Table 3

[0152]

[0153]

[0154]

[0155]

[0156] Combined with the test data in Table 3, it can be seen that the high-content water-soluble idebenone suspension inclusions prepared in Examples 1-7 have significantly better stability when used in skin care water than those in Comparative Examples 1-6.

[0157] Combining the test data in Tables 2 and 3, it can be seen that the stability of the high-content water-soluble idebenone suspension inclusions has a relatively large relationship with its stability after application in downstream products. The high-content water-soluble idebenone suspension inclusions have high stability and their application in downstream products also has high stability.

[0158] 3. Efficacy test: 130 volunteers were selected and divided into 13 groups, with 10 volunteers in each group, and each group of volunteers corresponded to one test sample.

[0159] The initial state of the volunteer's eye skin was photographed using the Antera3D multifunctional 3D skin imager, and the initial number of wrinkles was recorded. The test sample was then applied to the test area of ​​the tester, and after a half-hour interval, the eye skin state was photographed again (this was the 0.5h skin state), and the number of wrinkles at 0.5h was recorded. After 6 hours, the test sample was applied again, and after another half an hour, the eye skin state was photographed again (this was the 6.5h skin state), and the number of wrinkles at 6.5h was recorded.

[0160] The wrinkle reduction rate was calculated according to the following formula, and the average wrinkle reduction rate of the volunteers in the same group was taken as the test data of the group and recorded in Table 4.

[0161] Wrinkle count after use: 0.5h wrinkle count or 6.5h wrinkle count.

[0162] Table 4

[0163]

[0164] According to the comparison of the test data of Examples 1-3 and Comparative Examples 1-3 in Table 4, it can be seen that the wrinkle reduction rate of Comparative Examples 1-3 is not as high as that of Examples 1-3, which indicates that the combination of the specifically selected emulsifier, solubilizer and idebenone can form a stable inclusion body, and the use of idebenone in water-based products can give full play to the effect of idebenone and effectively eliminate wrinkles; if other raw materials are replaced or the specific combination is not used, the suspension inclusion body of idebenone cannot be formed, and its effect cannot be exerted.

[0165] According to the comparison of the test data of Examples 1-3 and Comparative Examples 4-6 in Table 4, it can be seen that after changing the process or process parameters of Example 1, the application effect of the high-content water-soluble idebenone suspension inclusions in the downstream water-based products will be affected. As for the reason why the performance of Comparative Example 5 is reduced despite the increase of the ultrasonic power, the inventors analyzed that it is because the excessively high ultrasonic frequency breaks the idebenone into too small a form. The skin care water is easy to evaporate, and the too small idebenone is dissipated due to the evaporation of the skin care water before it can fully play a role on the face, and cannot penetrate into the skin, resulting in poor anti-wrinkle effect.

[0166] One of them used the eye photo of the test sample of Example 1 for reference Fig.10 , one of them used the eye photo of the sample tested in Comparative Example 6 for reference Fig.11 .

[0167] In summary, under specific process conditions, the specially selected emulsifier, solubilizer and idebenone work together to form a special, uniform particle size, suitable size suspension inclusion, which can be well mixed with downstream water-based products and maintain the suspension and encapsulation effect. After the user applies the downstream water-based product, applying it with warm hands can more fully promote the skin to absorb the active substance.

[0168] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make modifications to the present embodiment without any creative contribution as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.

Claims

1. A high-content water-soluble idebenone suspension inclusion, characterized in that: According to the mass percentage, the raw materials include: 5-10% idebenone, 1-3% emulsifier, 5-15% solubilizer, 0.01-1% preservative, 15-25% alcohol solvent, and the solvent supplements the balance; The emulsifier is at least one or more of lecithin, hydrogenated lecithin, phosphatidylcholine, and a mixture of hydrogenated phosphatidylcholine; The solubilizer is dimethyl isosorbide, PPG-26-butanol polyether-26, cocoether-7, PPG-13-decyltetradecyl alcohol polyether-24, and diisopropyl sebacate. According to the mass percentage of the high-content water-soluble idebenone suspended inclusions, the mass percentage of dimethyl isosorbide is 4-6%, the mass percentage of PPG-26-butanol polyether-26 is 0.5-2%, the mass percentage of cocoether-7 is 1-2%, the mass percentage of PPG-13-decyltetradecyl alcohol polyether-24 is 1-2%, and the mass percentage of diisopropyl sebacate is 1.2-3.8%.

2. The high-content water-soluble idebenone suspension inclusion according to claim 1, characterized in that: The mass percentage of the solubilizer is 10-15%.

3. The high-content water-soluble idebenone suspension inclusion according to claim 1, characterized in that: The alcohol solvent is a mixture of one or more of glycerol, butanediol and pentanediol.

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