A ceramide complex, and a preparation method and application thereof
By using a water-in-oil emulsion drying method with a specific ratio of mannitol, starch, microcrystalline cellulose, and phospholipids to ceramides, the problems of poor dispersion and instability of ceramides in water have been solved, enabling their effective application in cosmetics and pharmaceuticals.
Patent Information
- Application Number
- CN202510095081.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-21
- Publication Date
- 2026-02-06
- Estimated Expiration
- 2045-01-21
AI Technical Summary
In the existing technology, ceramides are not easily soluble in water, making it difficult to disperse evenly in cosmetics. Furthermore, the stability of aqueous dispersions is poor, especially at high or low temperatures, which limits their widespread application.
A ceramide complex was prepared by using mannitol, starch, microcrystalline cellulose, phospholipids and ceramides in specific proportions via an oil-in-water emulsion drying method to form an oil-in-water solid, ensuring good water dispersibility and stability.
The prepared ceramide complex exhibits good dispersibility and high stability in water, effectively exerting its efficacy. It is also easy to package, store, and transport, and is not prone to deterioration, making it suitable for the preparation of cosmetics and pharmaceuticals.
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Figure CN119857091B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the cosmetic technology field, in particular to a ceramide compound and a preparation method and application thereof. BACKGROUND
[0002] At present, there are many excellent raw materials in the field of daily chemicals, such as ceramide substances, phytosphingosine substances and the like.
[0003] Ceramide is a kind of amide compound (mainly including ceramides 1-11) formed by long-chain fatty acid and sphingosine amino dehydration. Among them, ceramide 3 is obtained by acylating phytosphingosine and stearic acid, and ceramide 3B is synthesized by phytosphingosine and oleic acid. 40% to 50% of the sebum in the stratum corneum is composed of ceramide, and ceramide is the main part of the intercellular matrix, which plays an important role in maintaining the balance of water in the stratum corneum. Ceramide has a strong ability to associate with water molecules, and it maintains skin moisture by forming a network structure in the stratum corneum. Therefore, ceramide has the effect of maintaining skin moisture. Ceramides exist in all eukaryotic cells, and have important regulatory effects on cell differentiation, proliferation, apoptosis, aging and other life activities. As the main component of the intercellular lipid of the skin stratum corneum, ceramide not only acts as a second messenger molecule in the sphingomyelin pathway, but also plays an important role in the formation process of the epidermal stratum corneum, and has the effects of maintaining skin barrier, moisturizing, anti-aging, whitening and disease treatment.
[0004] However, most of the ceramide substances are not easy to dissolve in water, cannot be uniformly dispersed in water, and are easy to precipitate, which limits their wide application in the field of daily chemicals. For example, ceramide 3B or ceramide 3 cannot form a uniform solution when added to water, and solid precipitates are formed; when ceramide 3B or ceramide 3 is added to a cosmetic composition, precipitation also occurs, and when applied to the skin, it cannot be effectively absorbed by the skin, and cannot fully exert its efficacy.
[0005] At present, some preparation methods for increasing the water solubility or water dispersibility of these compounds (such as ceramide substances) that are not easy to dissolve in water have appeared in the prior art, but there are still some problems, such as that the initially prepared uniform ceramide aqueous dispersion liquid will precipitate after a period of time, and is unstable, and the stability of the ceramide aqueous dispersion liquid is poorer at high or low temperature.
[0006] In view of this, the present application is proposed. SUMMARY
[0007] The present application aims to provide a ceramide compound and a preparation method and application thereof, so as to solve or improve the above technical problems.
[0008] The present application can be implemented as follows:
[0009] In a first aspect, the present application provides a ceramide compound, which comprises 15-60 parts of a first component, 15-60 parts of a second component, 10-50 parts of a third component, 1-30 parts of a fourth component and 0.1-60 parts of a fifth component by mass fraction;
[0010] The first component comprises at least one of mannitol and lauryl maltitol ester;
[0011] The second component comprises starch;
[0012] The third component comprises microcrystalline cellulose;
[0013] The fourth component comprises a phospholipid compound;
[0014] The fifth component comprises a ceramide compound;
[0015] The ceramide compound is an oil-in-water solid.
[0016] In an optional embodiment, the ceramide compound comprises 15-40 parts of the first component, 15-40 parts of the second component, 10-30 parts of the third component, 1-20 parts of the fourth component and 0.1-50 parts of the fifth component.
[0017] In an optional embodiment, the ceramide compound comprises 24 parts of the first component, 23 parts of the second component, 15 parts of the third component, 7 parts of the fourth component and 28.58-31 parts of the fifth component.
[0018] In an optional embodiment, the starch comprises at least one of corn starch, malt dextrin and carboxymethyl starch;
[0019] And / or, the microcrystalline cellulose has a mesh number of 100-200;
[0020] And / or, the phospholipid compound comprises at least one of hydrogenated lecithin, lecithin, sunflower lecithin, phosphatidylcholine and phospholipid;
[0021] And / or, the ceramide compound is at least one of non-water-soluble ceramide and derivatives thereof.
[0022] In an optional embodiment, the ceramide compound comprises at least one of ceramide 3, ceramide 3B, ceramide EOP, ceramide AP and ceramide NS.
[0023] In an optional embodiment, the particle size of the ceramide compound is not more than 150 μm.
[0024] In a second aspect, the present application provides a method for preparing the ceramide complex according to any one of the preceding embodiments, comprising the following steps:
[0025] dispersing the first component, the second component and the third component in water to obtain a phase A;
[0026] dissolving the fourth component and the fifth component in an organic solvent to obtain a phase B;
[0027] pouring the phase B into the phase A to obtain an emulsion-like substance;
[0028] drying the emulsion-like substance to obtain the ceramide complex in solid form.
[0029] In an optional embodiment, the organic solvent comprises at least one of ethanol and a polyhydric alcohol;
[0030] In an optional embodiment, the polyhydric alcohol comprises at least one of ethylene glycol, propylene glycol and butylene glycol.
[0031] In an optional embodiment, when the organic solvent comprises both ethanol and a polyhydric alcohol, the mass of ethanol in the organic solvent is not less than 50wt%.
[0032] In an optional embodiment, after the phase B is poured into the phase A, the method further comprises the steps of homogenization, ultrasonication and stirring.
[0033] In an optional embodiment, the homogenization is performed at 5000rpm-12000rpm for 3min.
[0034] In an optional embodiment, the ultrasonication is performed at 200Hz-900Hz for 3min.
[0035] In an optional embodiment, the stirring is performed at 200rpm-2000rpm for 10min.
[0036] In an optional embodiment, the drying method comprises oven drying or spray drying.
[0037] In an optional embodiment, the spray drying is performed at an outlet temperature of 120℃-180℃ and a pump speed of 1%-20%.
[0038] In an optional embodiment, the spray drying is performed at an outlet temperature of 160℃ and a pump speed of 6%.
[0039] In a third aspect, the present application provides use of the ceramide complex according to any one of the preceding embodiments in the preparation of a daily-use chemical product or a pharmaceutical product.
[0040] In a fourth aspect, the present application provides a daily-use chemical product comprising the ceramide complex according to any one of the preceding embodiments.
[0041] In an optional embodiment, the daily chemical product is a cosmetic product.
[0042] In an optional embodiment, the cosmetic product comprises a facial cleanser, a skin care lotion, a skin care cream, a skin care milk, or a hair conditioner.
[0043] In an optional embodiment, the daily chemical product is in a dosage form comprising an ointment, a paste, a lotion, a gel, a solution, a suspension, an emulsion, a patch, or a spray.
[0044] In a fifth aspect, the present application provides a pharmaceutical product comprising the ceramide complex of any of the preceding embodiments.
[0045] In an optional embodiment, the pharmaceutical product is a pharmaceutical product for skin treatment.
[0046] In an optional embodiment, the pharmaceutical product is in a dosage form comprising an ointment, a paste, a lotion, a gel, a solution, a suspension, an emulsion, a patch, or a spray.
[0047] The beneficial effects of the present application include:
[0048] The ceramide complex prepared by compounding specific ingredients in specific proportions has good dispersibility in water and high stability of the aqueous dispersion. Moreover, the ceramide complex has a high content of ceramide compounds, which will not precipitate when added to subsequent formulations, and is beneficial to the efficacy of ceramide compounds when the product is prepared into a daily chemical product or a pharmaceutical product. In addition, the ceramide complex is in the form of an oil-in-water solid, which is convenient for packaging, storage, and transportation, has a long shelf life, and is not prone to spoilage. BRIEF DESCRIPTION OF DRAWINGS
[0049] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present application, and therefore should not be considered as limiting the scope. For those skilled in the art, other related drawings can also be obtained without creative labor.
[0050] Figure 1 Figure for the particle size test results of the ceramide complex of Example 1 in Test Example 1;
[0051] Figure 2 Figure for the particle size test results of the ceramide complex of Comparative Example 2 in Test Example 1;
[0052] Figure 3 Figure for the particle size test results of the ceramide complex of Comparative Example 3 in Test Example 1;
[0053] Figure 4Initial dispersion state diagram of the ceramide complex aqueous dispersion liquid prepared in Example 1 of Test Example 2 in which the mass fraction of the ceramide 3B was 0.3%;
[0054] Figure 5 Initial dispersion state diagram of the ceramide 3B aqueous dispersion liquid prepared in Example 1 of Test Example 2 in which the mass fraction of the ceramide 3B was 0.3%;
[0055] Figure 6 Initial dispersion state diagram of the ceramide complex aqueous dispersion liquid prepared in Example 1 of Test Example 2 in which the mass fraction of the ceramide 3B was 0.3%;
[0056] Figure 7 Dispersion result diagram of the ceramide complex in water prepared in Example 1 of Test Example 2;
[0057] Figure 8 Dispersion result diagram of the ceramide complex in water prepared in Example 1 of Test Example 2;
[0058] Figure 9 Dispersion result diagram of the ceramide complex in water prepared in Example 1 of Test Example 2;
[0059] Figure 10 State diagram of the ceramide complex aqueous dispersion liquid in which the mass fraction was 1% and 0.1% after being left at -20°C for half a month in Test Example 3;
[0060] Figure 11 State diagram of the ceramide complex aqueous dispersion liquid in which the mass fraction was 1% and 0.1% after being left at 4°C for half a month in Test Example 3;
[0061] Figure 12 State diagram of the ceramide complex aqueous dispersion liquid in which the mass fraction was 1% and 0.1% after being left at 45°C for half a month in Test Example 3. DETAILED DESCRIPTION
[0062] In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be described clearly and completely below. If specific conditions are not indicated in the embodiments, conventional conditions or conditions suggested by the manufacturers are adopted. If the reagents or instruments used are not indicated by the manufacturers, they are all conventional products that can be purchased in the market.
[0063] The ceramide complex provided by the present application and the preparation method and application thereof will be described in detail below.
[0064] The present application provides a ceramide compound, which comprises 15-60 parts of a first component, 15-60 parts of a second component, 10-50 parts of a third component, 1-30 parts of a fourth component, and 0.1-60 parts of a fifth component by mass fraction.
[0065] The first component comprises at least one of mannitol and lauryl maltitol ester, and mainly functions as an emulsifier.
[0066] The content of the first component in the ceramide compound can be 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, or 60 parts, or other values within the range of 15-60 parts.
[0067] The second component comprises starch, for example, at least one of corn starch, malt dextrin, and carboxymethyl starch. The second component mainly functions as a filler and a thickening agent.
[0068] The content of the second component in the ceramide compound can be 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, or 60 parts, or other values within the range of 15-60 parts.
[0069] The third component comprises microcrystalline cellulose, for example, the mesh number of the microcrystalline cellulose can be 100-200 mesh. The third component mainly functions as an emulsifier, a dispersant, and a thickening agent.
[0070] The content of the third component in the ceramide compound can be 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, or 50 parts, or other values within the range of 10-50 parts.
[0071] The fourth component comprises phospholipid compounds, for example, at least one of hydrogenated lecithin, lecithin, sunflower lecithin, phosphatidylcholine, and phospholipid. The fourth component mainly functions as an emulsifier and a carrier wrapping agent.
[0072] The content of the fourth component in the ceramide compound can be 1 part, 2 parts, 5 parts, 8 parts, 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, 22 parts, 25 parts, 28 parts, or 30 parts, or other values within the range of 1-30 parts.
[0073] The fifth component comprises ceramide compounds; the ceramide compounds are at least one of non-water-soluble ceramides and derivatives thereof, for example, at least one of ceramide 3, ceramide 3B, ceramide EOP, ceramide AP, and ceramide NS.
[0074] The content of the fifth component in the ceramide complex can be 0.1 part, 0.5 part, 1 part, 2 parts, 5 parts, 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts or 60 parts, etc., or other values in the range of 0.1 part to 60 parts. That is, in the present application, the ceramide complex can have good water dispersibility under the condition of containing a higher content of ceramide compounds.
[0075] In some preferred embodiments, the ceramide complex comprises 15 parts to 40 parts of the first component, 15 parts to 40 parts of the second component, 10 parts to 30 parts of the third component, 1 part to 20 parts of the fourth component, and 0.1 part to 50 parts of the fifth component. In some more typical embodiments, the ceramide complex comprises 24 parts of the first component, 23 parts of the second component, 15 parts of the third component, 7 parts of the fourth component, and 28.58 parts to 31 parts of the fifth component.
[0076] The ceramide complex under the above preferred ratio can have more optimal water dispersibility and stability.
[0077] In the present application, the particle size of the ceramide complex is not more than 150 μm, and is preferably concentrated in the range of 5.5 μm to 21.5 μm. Controlling the particle size of the ceramide complex in the above range can enable it to have excellent dispersion performance and stability after being dispersed in water.
[0078] In the present application, the ceramide complex is an oil-in-water type solid, which is beneficial to making the ceramide complex have good water dispersibility.
[0079] As described above, the ceramide complex provided in the present application has good dispersibility in water, and has high stability of the water dispersion. Moreover, the content of ceramide compounds in the complex is high, and the ceramide compounds will not be precipitated after being added to subsequent formula compositions, which is beneficial to the ceramide compounds to exert their efficacy after being prepared into daily-use products or medicines. For example, when the ceramide complex is used to prepare daily-use products, the ceramide compounds can enter the skin to exert their efficacy, enhance the skin barrier, and protect the skin against external stimuli.
[0080] It should be noted that in the prior art, a ceramide composition aqueous solution is prepared to improve the aqueous solution of ceramide compounds, but the content of ceramide in the above ceramide composition aqueous solution is low, not more than 10%, by adding more emulsifiers and other ingredients. Moreover, the ceramide composition aqueous solution is not convenient for storage, transportation and subsequent formula use. In the present application, the ceramide complex is set as an oil-in-water type solid, which is convenient for packaging, storage, transportation, has a long shelf life, and is not easy to deteriorate.
[0081] Correspondingly, the present application also provides a preparation method of the ceramide compound, comprising the following steps:
[0082] dispersing the first component, the second component and the third component in water to obtain phase A;
[0083] dissolving the fourth component and the fifth component in an organic solvent to obtain phase B;
[0084] pouring phase B into phase A to obtain an emulsion-like substance;
[0085] drying the emulsion-like substance to obtain the ceramide compound in solid form.
[0086] Through the above preparation sequence, the ceramide compound can have a suitable particle size, and can have excellent dispersion performance and stability in water.
[0087] In some embodiments, after phase B is poured into phase A, the method further comprises homogenization, ultrasonic treatment and stirring steps. The homogenization can be performed at 5000 rpm to 12000 rpm for 3 minutes, the ultrasonic treatment can be performed at 200 Hz to 900 Hz for 3 minutes, and the stirring can be performed at 200 rpm to 2000 rpm for 10 minutes.
[0088] In some alternative embodiments, the organic solvent can include at least one of ethanol and a polyhydric alcohol. The polyhydric alcohol can include at least one of ethylene glycol, propylene glycol and butylene glycol.
[0089] In some alternative embodiments, the drying method can include oven drying or spray drying.
[0090] The outlet temperature of the spray drying can be 120℃ to 180℃ (such as 120℃, 130℃, 140℃, 150℃, 160℃, 170℃ or 180℃, etc.), and the pump speed can be 1% to 20% (such as 1%, 2%, 5%, 8%, 15% or 20%, etc.). In some typical embodiments, the outlet temperature of the spray drying is 160℃, and the pump speed is 6%.
[0091] In addition, the present application also provides a use of the ceramide compound in the preparation of daily-use chemicals or medicines.
[0092] Correspondingly, the present application also provides a daily-use chemical containing the ceramide compound.
[0093] In some alternative embodiments, the daily-use chemical is a cosmetic, which can exemplarily but non-limitingly include facial cleanser, skin care water, skin care milk, skin care cream or hair conditioner, etc.
[0094] In some alternative embodiments, the dosage form of the daily-use cosmetic can exemplarily but non-limitatively include an ointment, a paste, a lotion, a gel, a solution, a suspension, an emulsion, a patch, or a spray, etc.
[0095] Accordingly, the present application also provides a pharmaceutical product containing the ceramide complex.
[0096] In some alternative embodiments, the pharmaceutical product is a pharmaceutical product for skin treatment.
[0097] Similarly, the dosage form of the pharmaceutical product can exemplarily but non-limitatively include an ointment, a paste, a lotion, a gel, a solution, a suspension, an emulsion, a patch, or a spray.
[0098] By using the ceramide complex provided by the present application in daily-use cosmetics or pharmaceutical products, the ceramide can effectively exert its efficacy.
[0099] The features and performances of the present application are further described in detail below in combination with examples.
[0100] Example 1
[0101] The present example provides a ceramide complex, which includes 24 parts of mannitol, 23 parts of corn starch, 15 parts of microcrystalline cellulose, 7 parts of hydrogenated lecithin, and 31 parts of ceramide 3B by weight.
[0102] The preparation of the ceramide complex includes:
[0103] S1: 2.4 g of mannitol, 2.3 g of corn starch, and 1.5 g of microcrystalline cellulose are weighed and dispersed in 100 mL of 70°C water as a wall material to obtain phase A;
[0104] S2: 0.7 g of hydrogenated lecithin and 3.1 g of ceramide 3B are weighed and dissolved in 100 mL of 70°C ethanol as a core material to obtain phase B;
[0105] S3: The phase B is poured into the phase A, homogenized at 10,000 rpm for 3 min, then ultrasonically treated at 400 Hz for 3 min, and finally stirred at 200 rpm for 10 min to obtain an emulsion-like substance;
[0106] S4: The emulsion-like substance is dried at 60°C to obtain a ceramide complex in the form of white powder.
[0107] Example 2
[0108] The embodiment provides a ceramide compound, which comprises 24 parts of mannitol, 23 parts of corn starch, 15 parts of microcrystalline cellulose, 7 parts of hydrogenated lecithin, 20 parts of ceramide 3B, 8.1 parts of ceramide AP and 0.48 parts of ceramide EOP in terms of weight parts.
[0109] The preparation of the ceramide compound comprises the following steps:
[0110] S1: 2.4 g of mannitol, 2.3 g of corn starch and 1.5 g of microcrystalline cellulose are weighed and dispersed in 100 mL of 70 DEG C water as wall materials to obtain phase A;
[0111] S2: 0.7 g of hydrogenated lecithin, 2 g of ceramide 3B, 0.81 g of ceramide AP and 0.048 g of ceramide EOP are weighed and dissolved in 100 mL of 70 DEG C ethanol as core materials to obtain phase B;
[0112] S3: the phase B is poured into the phase A, homogenized at 10000 rpm for 3 min, then ultrasonically treated at 400 Hz for 3 min, and finally stirred at 200 rpm for 10 min to obtain an emulsion-like substance;
[0113] S4: the emulsion-like substance is dried at 60 DEG C to obtain a ceramide compound in the form of white powder.
[0114] Embodiment 3
[0115] The embodiment provides a ceramide compound, which comprises 24 parts of mannitol, 23 parts of corn starch, 15 parts of microcrystalline cellulose, 7 parts of hydrogenated lecithin, 20 parts of ceramide 3B, 8.1 parts of ceramide AP and 0.48 parts of ceramide EOP in terms of weight parts.
[0116] The preparation of the ceramide compound comprises the following steps:
[0117] S1: 2.4 g of mannitol, 2.3 g of corn starch and 1.5 g of microcrystalline cellulose are weighed and dispersed in 100 mL of 70 DEG C water as wall materials to obtain phase A;
[0118] S2: 0.7 g of hydrogenated lecithin, 2 g of ceramide 3B, 0.81 g of ceramide AP and 0.048 g of ceramide EOP are weighed and dissolved in 100 mL of 70 DEG C ethanol as core materials to obtain phase B;
[0119] S3: the phase B is poured into the phase A, homogenized at 10000 rpm for 3 min, then ultrasonically treated at 400 Hz for 3 min, and finally stirred at 200 rpm for 10 min to obtain an emulsion-like substance;
[0120] S4: The emulsion-like substance was dried at 60°C to obtain a white powdery ceramide complex.
[0121] Example 4
[0122] This example provides a ceramide complex, which includes 24 parts of mannitol, 23 parts of corn starch, 15 parts of microcrystalline cellulose, 7 parts of hydrogenated lecithin, and 31 parts of ceramide 3B by weight.
[0123] The preparation of the ceramide complex includes:
[0124] S1: 2.4 g of mannitol, 2.3 g of corn starch, and 1.5 g of microcrystalline cellulose were weighed and dispersed in 100 mL of 70°C water as a wall material to obtain phase A;
[0125] S2: 0.7 g of hydrogenated lecithin and 3.1 g of ceramide 3B were weighed and dissolved in 100 mL of 70°C ethanol as a core material to obtain phase B;
[0126] S3: The above phase B was poured into phase A, homogenized at 10,000 rpm for 3 min, then ultrasonicated at 400 Hz for 3 min, and stirred at 200 rpm for 10 min to obtain an emulsion-like substance;
[0127] S4: The emulsion-like substance was spray dried at a pump speed of 6% and an outlet temperature of 160°C to obtain a white powdery ceramide complex.
[0128] Comparative Example 1
[0129] The difference between this comparative example and Example 1 is the preparation process (the amounts and substances of the components are the same), specifically, in S1, the mannitol, corn starch, microcrystalline cellulose, and hydrogenated lecithin are collectively used as phase A; in S2, only ceramide 3B is used as phase B; S3 and S4 are the same as Example 1.
[0130] Comparative Example 2
[0131] The difference between this comparative example and Example 1 is the preparation process (the amounts and substances of the components are the same), specifically, in S1, the mannitol and corn starch are collectively used as phase A; in S2, the microcrystalline cellulose, hydrogenated lecithin, and ceramide 3B are collectively used as phase B; S3 and S4 are the same as Example 1.
[0132] Comparative Example 3
[0133] The difference between this comparative example and Example 1 lies in the preparation process (the amount and substances of each component are the same). Specifically, in S1, corn starch and microcrystalline cellulose are used together as phase A; in S2, mannitol, hydrogenated lecithin and ceramide 3B are used together as phase B; S3 and S4 are the same as in Example 1.
[0134] Experimental Example 1
[0135] Since the ceramide complex prepared in Comparative Example 1 could not be uniformly dispersed, the particle size of the ceramide complexes prepared in Example 1 and Comparative Examples 1-2 was tested in this experiment. The test was conducted by the Analysis and Testing Center of Jiangxi Academy of Sciences and the results were provided.
[0136] The particle size test results of the ceramide complex in Example 1 are as follows: Figure 1 As shown, by Figure 1 It can be seen that the particle size of the ceramide complex in Example 1 is in the range of 0.0529 μm to 149 μm, and is more concentrated in the range of 5.5 μm to 21.5 μm.
[0137] The particle size test results of the ceramide complex in Comparative Example 2 are as follows: Figure 2 As shown, by Figure 3 It can be seen that the particle size of the ceramide complex in Comparative Example 2 is in the range of 1.59 μm to 286 μm, and is more concentrated in the range of 13.1 μm to 66.4 μm.
[0138] The particle size distribution results of the ceramide complex in Comparative Example 3 are as follows: Figure 4 As shown, by Figure 4 It can be seen that the particle size of the ceramide complex in Comparative Example 3 is in the range of 0.370 μm to 176 μm, and is more concentrated in the range of 8.07 μm to 25.1 μm.
[0139] The test results above show that, in terms of dispersion particle size, the water dispersibility of the ceramide complex prepared in Example 1 of this invention is better than that of Comparative Example 2 and Comparative Example 3.
[0140] Furthermore, tests showed that the particle size of the ceramide complexes prepared in Examples 2-4 of this invention did not exceed 150 μm.
[0141] Experimental Example 2
[0142] ① Water dispersibility test of ceramide complex
[0143] The ceramide complex obtained in Example 1 was dispersed in water to prepare an aqueous dispersion of the ceramide complex with a mass fraction of 0.3% ceramide 3B. The initial dispersion state of this aqueous dispersion of the ceramide complex is as follows: Figure 4 As shown.
[0144] Depend on Figure 4 It can be seen that the ceramide complex prepared in Example 1 can be uniformly dispersed in water.
[0145] A 0.3% (w / w) aqueous dispersion of ceramide 3B was used as a control. The preparation of this 0.3% (w / w) aqueous dispersion of ceramide 3B was as follows: Ceramide 3B was added to water and stirred to obtain a 0.3% (w / w) aqueous dispersion of ceramide 3B. The initial dispersion state of this 0.3% (w / w) aqueous dispersion was as follows: Figure 5 As shown.
[0146] Depend on Figure 5 It can be seen that a large amount of precipitate exists in the 0.3% (w / w) aqueous dispersion of ceramide 3B. Furthermore, as the concentration of ceramide 3B increases, even more precipitate forms in the aqueous solution.
[0147] By comparison Figure 4 and Figure 5 It can be seen that, at the same effective concentration, the ceramide complex prepared according to Example 1 of this application and redispersed in water exhibits better water dispersibility than when directly added to water.
[0148] Further, the ceramide complex obtained in Comparative Example 3 was dispersed in water to prepare an aqueous dispersion of the ceramide complex with a mass fraction of 0.5%. The initial dispersion state of this aqueous dispersion of the ceramide complex is as follows: Figure 6 As shown.
[0149] Depend on Figure 4 and Figure 6 The comparison shows that the ceramide complex in Comparative Example 3 has significantly worse dispersibility in water than the ceramide complex in Example 1 within the particle size range.
[0150] ② Dispersed comparison test
[0151] Weigh 1g of the ceramide complex prepared in Comparative Example 1 into a beaker, add 1% pure water by mass, and magnetically stir at 200rpm / min for 3 minutes at room temperature. The mixture failed to disperse, exhibiting particle aggregation, stratification, and other unevenness. At 60℃, stirring at 200rpm / min for 30 minutes resulted in further failure to disperse, and after standing, stratification and precipitation occurred. Figure 7 As shown. By Figure 7 It can be seen that the ceramide complex prepared in Comparative Example 1 has poor water dispersibility and cannot be uniformly dispersed.
[0152] The water dispersibility of the ceramide complex prepared in Comparative Example 2 was tested using the same method as in Comparative Example 1, and the results are as follows: Figure 8 As shown, byFigure 8 It can be seen that the water dispersibility of the ceramide complex prepared in Comparative Example 2 is also poor.
[0153] The water dispersibility of the ceramide complex prepared in Comparative Example 3 was tested in the same manner as in Comparative Example 1, and the results are shown in Table 1. Figure 9 Figure 9 It can be seen that the water dispersibility of the ceramide complex prepared in Comparative Example 3 is also poor.
[0154] Test Example 3
[0155] Stability test of ceramide complex water dispersion
[0156] The ceramide complex prepared in Example 1 was dispersed in water to prepare ceramide complex water dispersions having a mass fraction of 1% and 0.1%, respectively. The ceramide complex water dispersions having a mass fraction of 1% and 0.1% were placed at -20°C, and the state after half a month was as shown in Figs. 2(a) and 2(b), respectively. As can be seen from Figs. 2(a) and 2(b), the ceramide complex water dispersions having a mass fraction of 1% and 0.1% were stable without precipitation and stratification after half a month at -20°C. Figure 10 Figure 10 Figure 10 As can be seen, the ceramide complex water dispersions having a mass fraction of 1% and 0.1% were stable without precipitation and stratification after half a month at -20°C.
[0157] The ceramide complex prepared in Example 1 was dispersed in water to prepare ceramide complex water dispersions having a mass fraction of 1% and 0.1%, respectively. The ceramide complex water dispersions having a mass fraction of 1% and 0.1% were placed at 4°C, and the state after half a month was as shown in Figs. 3(a) and 3(b), respectively. As can be seen from Figs. 3(a) and 3(b), the ceramide complex water dispersions having a mass fraction of 1% and 0.1% were stable without precipitation and stratification after half a month at 4°C. Figure 11 Figure 11 Figure 11 As can be seen, the ceramide complex water dispersions having a mass fraction of 1% and 0.1% were stable without precipitation and stratification after half a month at 4°C.
[0158] The ceramide complex prepared in Example 1 was dispersed in water to prepare ceramide complex water dispersions having a mass fraction of 1% and 0.1%, respectively. The ceramide complex water dispersions having a mass fraction of 1% and 0.1% were placed at 45°C, and the state after half a month was as shown in Figs. 4(a) and 4(b), respectively. As can be seen from Figs. 4(a) and 4(b), the ceramide complex water dispersions having a mass fraction of 1% and 0.1% were stable without precipitation and stratification after half a month at 45°C. Figure 12 Figure 12 Figure 12 As can be seen, the ceramide complex water dispersions having a mass fraction of 1% and 0.1% were stable without precipitation and stratification after half a month at 45°C.
[0159] In addition, the ceramide complexes prepared in Examples 2 to 4 also have excellent dispersibility and stability in water.
[0160] Application Example
[0161] The ceramide complex prepared in Example 1 was prepared into an emulsion according to the formulation in Table 1.
[0162] Table 1 Emulsion Formulation
[0163]
[0164]
[0165] The preparation method of the above emulsion is as follows:
[0166] Phase A: weigh each component in beaker 1 according to Table 1, add pure water, and stir uniformly at 70-90℃;
[0167] Phase B: weigh each component in beaker 2 according to Table 1, melt into a uniform oily liquid at 70-90℃;
[0168] Phase C: weigh each component in beaker 3 according to Table 1, add pure water, and stir to dissolve;
[0169] Pour phase B into phase A, homogenize at 90℃ for 10 min, after homogenization, stir at 200 rpm for 30 min to room temperature, pour phase C into the above mixture, continue to stir for 10 min, and obtain the emulsion.
[0170] The emulsion prepared according to the formulation in Table 1 has a relatively delicate skin feel, is easy to push away and absorb, has good moisturizing property and permeability, is beneficial to the absorption of the skin, and is beneficial to the full play of the efficacy of the effective component (ceramide).
[0171] In summary, the scheme provided by the present application has at least the following advantages:
[0172] (1) The preparation method of the ceramide complex provided by the present application is reasonable, and can prepare a complex powder with small and uniform particle size, and the content of the effective component (ceramide compound) in the complex powder is high.
[0173] (2) The ceramide complex provided by the present application has good water dispersibility, and has high stability. When it is added to the subsequent formulation composition, it will not precipitate, which is beneficial to the ceramide compound to enter the skin to play its efficacy, enhance the skin barrier, protect the skin, and resist some external stimuli.
[0174] (3) The ceramide complex provided by the present application is convenient for packaging, storage and transportation, is relatively stable and not easy to deteriorate, and is easy to use and develop in subsequent formulations.
[0175] (4) The ceramide complex provided by the application has a high content of effective components (ceramide compounds), up to about 60%, and does not introduce too many other substances, and does not affect the preparation of subsequent formulations.
[0176] The above merely provides the preferred embodiments of the application, but should not be used to limit the application, and various modifications and changes can be made by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the application should be included in the protection scope of the application.
Claims
1. A ceramide complex, characterized by, The ceramide complex comprises 15-60 parts by mass of the first component, 15-60 parts by mass of the second component, 10-50 parts by mass of the third component, 1-30 parts by mass of the fourth component, and 0.1-60 parts by mass of the fifth component; The first component comprises at least one of mannitol and lauryl maltitol ester; The second component comprises starch; The third component comprises microcrystalline cellulose; The fourth component comprises phospholipid compounds; The fifth component comprises ceramide compounds; The ceramide complex is in the form of solid oil-in-water; The preparation method of the ceramide complex comprises the following steps: The first component, the second component, and the third component are dispersed in water to obtain phase A; The fourth component and the fifth component are dissolved in an organic solvent to obtain phase B; the organic solvent is ethanol; The phase B is poured into the phase A to obtain an emulsion-like substance in the form of oil-in-water; The emulsion-like substance is dried to obtain the ceramide complex in the form of solid.
2. The ceramide complex according to claim 1, characterized in that, The ceramide complex comprises 15-40 parts by mass of the first component, 15-40 parts by mass of the second component, 10-30 parts by mass of the third component, 1-20 parts by mass of the fourth component, and 0.1-50 parts by mass of the fifth component.
3. The ceramide complex according to claim 2, characterized in that, The ceramide complex comprises 24 parts of the first component, 23 parts of the second component, 15 parts of the third component, 7 parts of the fourth component, and 28.58-31 parts of the fifth component.
4. The ceramide complex according to any one of claims 1 to 3, characterized in that, The starch comprises at least one of corn starch, malt dextrin, and carboxymethyl starch; And / or, the mesh number of the microcrystalline cellulose is 100-200; And / or, the phospholipid compounds comprise at least one of hydrogenated lecithin, lecithin, sunflower lecithin, phosphatidylcholine, and phospholipid; And / or, the ceramide compounds are at least one of non-water-soluble ceramides and derivatives thereof.
5. The ceramide complex according to claim 4, characterized in that, The ceramide compounds comprise at least one of ceramide 3, ceramide 3B, ceramide EOP, ceramide AP, and ceramide NS.
6. The ceramide complex according to any one of claims 1 to 3, characterized in that, The particle size of the ceramide complex is not more than 150 μm.
7. A process for the preparation of a ceramide complex according to any one of claims 1 to 6, characterized in that, The preparation method comprises the following steps: The first component, the second component, and the third component are dispersed in water to obtain phase A; The fourth component and the fifth component are dissolved in an organic solvent to obtain phase B; the organic solvent is ethanol; The phase B is poured into the phase A to obtain an emulsion-like substance in the form of oil-in-water; The emulsion-like substance is dried to obtain the ceramide complex in the form of solid.
8. The production method according to claim 7, characterized by, After the phase B is poured into the phase A, the steps of homogenization, ultrasonic treatment, and stirring are further included; And / or, the drying method comprises baking or spray drying.
9. The production method according to claim 8, characterized by, The homogenization is performed at 5000-12000 rpm for 3 min.
10. The preparation method according to claim 8, characterized in that, The ultrasonic treatment is performed at 200-900 Hz for 3 min.
11. The preparation method according to claim 8, characterized in that, The stirring is performed at 200-2000 rpm for 10 min.
12. The method of claim 8, wherein, The outlet temperature of the spray drying is 120-180°C, and the pump speed is 1-20%.
13. The preparation method according to claim 8, characterized in that, The outlet temperature of the spray drying was 160°C and the pump speed was 6%.
14. Use of the ceramide complex according to any one of claims 1 to 6 for the manufacture of a cosmetic or pharmaceutical product.
15. A daily use cosmetic product, characterized by, The cosmetic product comprises the ceramide complex according to any one of claims 1 to 6.
16. The personal care product of claim 15, wherein, The cosmetic product is a cosmetic.
17. The personal care product of claim 16, wherein, The cosmetic comprises a facial cleanser, a skin care lotion, a skin care cream, or a hair conditioner.
18. The personal care product of claim 16, wherein, The cosmetic product is in the form of an ointment, a paste, a lotion, a gel, a solution, a suspension, an emulsion, a patch, or a spray.
19. A medicine, characterized in that, The pharmaceutical product comprises the ceramide complex according to any one of claims 1 to 6.
20. The pharmaceutical product according to claim 19, characterized in that The pharmaceutical product is a pharmaceutical product for the treatment of the skin.
21. The pharmaceutical product according to claim 20, characterized in that The pharmaceutical product is in the form of an ointment, a paste, a lotion, a gel, a solution, a suspension, an emulsion, a patch, or a spray.
Citation Information
Patent Citations
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