Collagen-containing microcapsule emulsion and preparation method thereof
By adjusting the pH value and Zeta potential value of the collagen solution, it solves the problem of difficult collagen absorption and wrapping, and achieves its efficient penetration and sustained release on the skin, improving the whitening effect and simplifying the process.
Patent Information
- Application Number
- CN202411444810.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-16
- Publication Date
- 2025-01-10
- Estimated Expiration
- 2044-10-16
AI Technical Summary
In the prior art, collagen is difficult to absorb by the skin, resulting in waste of light or microbial decomposition on the skin surface, and conventional preparations are difficult to achieve effective wrapping and sustained release of electrodual collagen.
By adjusting the pH value and Zeta potential value of the collagen solution, it forms microcapsules in the isoelectric point state, and synergistically synergistically with collagen is achieved to improve the stability and transdermal absorption of collagen, and The bioavailability and sustained release effect are improved by the preparation method of microcapsule emulsion.
It successfully improves the transdermal absorption effect and stability of collagen, makes up for the shortcomings of insufficient whitening effect, simplifies the process, and avoids complex preparation methods and high-cost solvent use.
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Figure CN119280103A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of cosmetic preparations, and particularly relates to a microcapsule emulsion containing collagen and a preparation method thereof. Background Art
[0002] As we age, long-term exposure to ultraviolet rays, irregular work and rest, and malnutrition can easily cause the loss of collagen in the human body, leading to skin aging. With the loss of a large amount of collagen, the skin gradually undergoes structural changes and functional decline, showing obvious characteristics of skin aging such as decreased skin elasticity, sagging skin, wrinkles and fine lines, pigmentation, dryness, roughness, and sensitivity.
[0003] Adding collagen to cosmetics can effectively supplement the loss of collagen in the skin. Collagen raw materials are now increasingly used in cosmetic formulas. As a safe ingredient with multiple functions such as anti-aging and moisturizing, how to improve its utilization efficiency and exert its efficacy is the starting point of the research of this application. Studies in the prior art have found that macromolecular collagen is difficult to be absorbed by the skin, and consumers are also very concerned about whether the collagen added to the formula can really play a role through the skin. If the collagen directly added to the formula system cannot be absorbed by the skin, it may be wasted on the skin surface through light or microbial decomposition. Since collagen for external use on the skin generally has the problem of being difficult to fully absorb, collagen peptides prepared by enzymatic hydrolysis are usually used for external use on the skin. Collagen peptides have a smaller molecular weight and are more easily absorbed through the skin. The collagen used in this application is all small molecule collagen peptide raw materials.
[0004] In addition, the problem of transdermal absorption can be solved by formulation encapsulation technology to improve the bioavailability of collagen and exert the sustained release effect of collagen. However, the carboxyl and amino groups of collagen itself are amphoteric in aqueous solution, and carry different charges according to the pH value of the solution, so it is difficult to achieve the encapsulation of bi-charged collagen by conventional formulation methods.
[0005] For example, Chinese patent application CN202311025794 discloses an anti-hair loss stock solution containing transdermal recombinant collagen and a preparation method thereof. This technical method uses recombinant collagen with skin affinity and tissue compatibility as the basic component, and uses glycerol encapsulation technology to encapsulate highly active recombinant collagen in glycerol body vesicles, so that it has the characteristics of high stability, controlled sustained release, safety and mildness. However, this technical method introduces ethanol as an organic solvent, and uses ultrasound and other processes at the same time, which has complex processes and cumbersome production processes. Chinese patent application CN202410583047 discloses a supramolecular collagen microcapsule suitable for sensitive skin and its preparation method and application. This technology uses low eutectic solvent technology to compound dipalmitoyl hydroxyproline and bisabolol to prepare a new type of low eutectic solvent, which can effectively encapsulate and deliver the composite protein to form a system-stable supramolecular microcapsule, effectively improving the protein encapsulation rate, thereby achieving the advantages of efficient penetration and targeted delivery of the composite protein on the skin. However, this technical method has disadvantages such as a relatively complicated process for preparing a low eutectic solvent, requiring light protection or nitrogen protection, and a long reaction time.
[0006] In view of this, it is necessary to develop a new microcapsule emulsion containing collagen so as to maximize the efficacy of collagen. Summary of the invention
[0007] In order to overcome the defects and deficiencies in the prior art, the present invention provides a microcapsule emulsion containing collagen and a preparation method thereof. The present invention innovatively uses tranexamic acid to adjust the pH value and Zeta potential value of the collagen solution system, so that the collagen exhibits the characteristics of the lowest solubility and the lowest conductivity when it is close to the isoelectric point, and successfully prepares a microcapsule preparation containing collagen, thereby achieving improved collagen stability and transdermal absorbability, as well as sustained release to improve skin condition.
[0008] The purpose of the present invention can be achieved through the following technical solutions:
[0009] In a first aspect, the present invention provides a method for preparing microcapsules containing collagen, the preparation method comprising the following steps:
[0010] (1) Add 0.01-1 g acetic acid or formic acid to 10-100 g water, add 0.1-5 g chitosan until it is completely dissolved, then dissolve 0.02-2 g surfactant and 0.1-5 g calcium chloride, and homogenize until no obvious particles are formed to form solution A;
[0011] (2) Dissolve 0.1-5 g collagen and 0.1-1 g tranexamic acid in 5-50 g water and disperse them evenly in the water to form solution B;
[0012] (3) Pre-dissolve 2 g of sodium alginate in 5-50 g of water until it is completely dissolved to form solution C;
[0013] (4) Add solution B and solution C to solution A at a dropping speed of 0.01-0.1 g / s at the same time, homogenizing at a speed of 5000-10000 rpm, to form solution D, i.e., a microcapsule solution containing collagen.
[0014] As an optional mode, in the above preparation method, the preparation method comprises the following steps:
[0015] (1) Add 0.1-0.5 g acetic acid or formic acid to 30-80 g water, add 0.5-2 g chitosan until completely dissolved, then dissolve 0.2-1 g surfactant and 0.5-2 g calcium chloride, and homogenize until no obvious particles are formed to form solution A;
[0016] (2) Dissolve 0.5-2 g collagen and 0.5-1 g tranexamic acid in 10-30 g water and disperse them evenly in the water to form solution B;
[0017] (3) Pre-dissolve 2 g of sodium alginate in 10-30 g of water until it is completely dissolved to form solution C;
[0018] (4) Add solution B and solution C to solution A at a dropping speed of 0.02-0.08 g / s while homogenizing at a speed of 7000-10000 rpm to form solution D, i.e., a microcapsule solution containing collagen.
[0019] As an optional manner, in the above preparation method, the preparation method comprises the following steps: the surfactant is selected from one or more of the following: Tween-80, Span-80, monoglyceride of fatty acid or sucrose ester of fatty acid.
[0020] Preferably, in the above preparation method, in step (1), 0.01-1 g of Tween-80 and 0.01-1 g of Span-80 are used as surfactants.
[0021] More preferably, in the above preparation method, in step (1), 0.1-0.5 g of Tween-80 and 0.1-0.5 g of Span-80 are used as surfactants.
[0022] As an optional mode, in the preparation method of the present invention, the collagen used is derived from fish skin and has a molecular weight of less than 1000Da.
[0023] In a second aspect, the present invention provides microcapsules containing collagen prepared by the preparation method described in the first aspect.
[0024] In a third aspect, the present invention provides a method for preparing a microcapsule emulsion containing collagen, the preparation method comprising the following steps:
[0025] (1) taking 50-150 g of the collagen microcapsule solution described in the second aspect, pre-dissolve 0.1-5 g of glycerol and 0.1-15 g of polyol until they are completely dissolved to form solution A;
[0026] (2) dissolving 0.1-5 g of cetearyl glucoside or glyceryl stearate in 1-10 g of fat and uniformly dispersing at 70-90° C. to form solution B;
[0027] (3) Add solution B to solution A and homogenize at a speed of 5000-10000 rpm to form an emulsion sample, i.e., a microcapsule emulsion containing collagen.
[0028] As an optional mode, in the above preparation method, the preparation method comprises the following steps:
[0029] (1) taking 80-120 g of the collagen microcapsule solution described in the second aspect, pre-dissolve 0.5-2 g of glycerol and 0.5-10 g of polyol until they are completely dissolved to form solution A;
[0030] (2) dissolving 0.5-2 g of cetearyl glucoside or glyceryl stearate in 1-10 g of caprylic capric triglyceride or jojoba oil, and dispersing the mixture evenly at 80° C. to form a solution B;
[0031] (3) Add solution B to solution A and homogenize at a speed of 7000-10000 rpm to form an emulsion sample, i.e., a microcapsule emulsion containing collagen.
[0032] As an optional manner, in the above preparation method, in step (1), the polyol is selected from one or more of the following: propylene glycol, butylene glycol or pentanediol.
[0033] Preferably, in the above preparation method, in step (1), 0.1-5 g of butanediol and 1-10 g of pentanediol are used as polyols.
[0034] More preferably, in the above preparation method, in step (1), 0.5-2 g of glycerol and 0.5-2 g of butanediol are used as polyols.
[0035] In a fourth aspect, the present invention provides a microcapsule emulsion containing collagen prepared by the preparation method described in the third aspect.
[0036] In a fifth aspect, the present invention provides use of the microcapsules containing collagen described in the second aspect or the microcapsule emulsion containing collagen described in the fourth aspect in the preparation of cosmetics.
[0037] As an optional mode, in the above-mentioned use, the cosmetic is toner, lotion, essence, cream, ointment, facial mask or freeze-dried powder.
[0038] Compared with the prior art, the present invention has the following beneficial effects:
[0039] (1) Since collagen has dual charge, it is difficult to achieve cross-linking and encapsulation of collagen using conventional microencapsulation methods. This application uses the isoelectric point of collagen to achieve cross-linking and encapsulation of collagen. The process is simple and can be achieved using conventional equipment and experimental conditions.
[0040] (2) The pH value and Zeta potential value are adjusted by tranexamic acid so that the collagen can be prepared in the isoelectric state. The synergistic effect of tranexamic acid and collagen is brought into play, which makes up for the shortcoming of collagen's insufficient whitening effect.
[0041] (3) The preparation of microcapsules was achieved by cross-linking and encapsulating collagen, which effectively improved the transdermal absorption effect of collagen. BRIEF DESCRIPTION OF THE DRAWINGS
[0042] Figure 1 : Microscopic photograph of the collagen-containing microcapsules prepared by the method of Example 1.
[0043] Figure 2 : Comparison of the permeability of microcapsule emulsion containing collagen (sample 1) and ordinary emulsion containing collagen (sample 2).
[0044] Figure 3 : Sample photos of microcapsules containing collagen prepared by the methods of Example 1 and Comparative Examples 1-6. From left to right are Comparative Examples 1-6 and Example 1. DETAILED DESCRIPTION
[0045] The present invention will be further described with reference to specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the scope of the present invention.
[0046] If no specific techniques or conditions are specified in the examples, the techniques or conditions described in the literature in the field or the product instructions are used. If no manufacturer is specified for the reagents or instruments used, they are all conventional products that can be purchased through regular channels.
[0047] The experimental methods in the following examples are conventional methods unless otherwise specified. The experimental materials used in the following examples are commercially available products unless otherwise specified.
[0048] Example 1: Preparation of microcapsules containing collagen of the present invention
[0049] (1) Add 0.2 g acetic acid to 60 g water, add 1 g chitosan until completely dissolved, then dissolve 0.2 g Tween-80, 0.2 g Span-80, and 1 g calcium chloride and homogenize until no obvious particles are formed to form solution A;
[0050] (2) Dissolve 1 g of collagen (derived from fish skin, with a molecular weight of less than 1000 Da, and the following collagen indicators are the same) and 0.7 g of tranexamic acid in 20 g of water, and uniformly disperse them in the water to form solution B;
[0051] (3) Pre-dissolve 2 g of sodium alginate in 20 g of water until it is completely dissolved to form solution C;
[0052] (4) Solution B and Solution C were added dropwise to Solution A at a dropping speed of 0.05 g / s while being homogenized at a speed of 8000 rpm to form Solution D, i.e., a microcapsule solution containing collagen.
[0053] The pH value of the collagen-containing microcapsule solution was 6.8, and the Zeta potential value was -10.58 mV.
[0054] Literature research and experimental results show that anionic sodium alginate is complexed with cationic chitosan through electrostatic interaction, and collagen is cross-linked to the sodium alginate interface layer through hydrogen bonds. There are also studies reporting that heating and acidic conditions can induce chitosan and collagen to form a complex through hydrogen bonds, and the sodium alginate and chitosan complex formed by electrostatic interaction undergoes interfacial self-assembly into capsules. At the same time, collagen further enhances the mechanical stability of the capsule through hydrogen bonds, thereby improving the overall compressive resistance of the microcapsules.
[0055] It was found in the experiment that due to the active charge characteristics of collagen, a stable potential interface is required under specific pH conditions to facilitate the stable existence of sodium alginate chitosan capsules, especially for capsules formed by positive and negative charge adsorption, which are particularly sensitive to environmental charge stability. The isoelectric point of collagen obtained by different processes may be different, and the pH value and Zeta potential value need to be determined by experimental exploration.
[0056] The microcapsule samples prepared by the above method are shown in the following microscope photos: Figure 1 shown. Figure 1The microscopic photograph in the figure was obtained using a fluorescent inverted microscope with a magnification of 200 times. It can be seen from the photograph that the microcapsules are uniform and stable, there is no obvious adhesion between the microcapsules, and the average particle size of the microcapsules is about 10 μm.
[0057] Comparative Example 1: Preparation of microcapsules containing collagen without tranexamic acid
[0058] (1) Add 0.2 g acetic acid to 60 g water, add 1 g chitosan until completely dissolved, then dissolve 0.2 g Tween-80, 0.2 g Span-80, and 1 g calcium chloride and homogenize until no obvious particles are formed to form solution A;
[0059] (2) Dissolve 1 g of collagen in 20 g of water and disperse it evenly in the water to form solution B;
[0060] (3) Pre-dissolve 2 g of sodium alginate in 20 g of water until it is completely dissolved to form solution C;
[0061] (4) Solution B and Solution C were added dropwise to Solution A at a dropping speed of 0.05 g / s while being homogenized at a speed of 8000 rpm to form Solution D, i.e., a microcapsule solution containing collagen.
[0062] The pH value of the microcapsule solution containing collagen was 3.8, and the Zeta potential value was -2.17 mV. It was observed that the microcapsule solution sample was obviously flocculated.
[0063] Comparative Example 2: Preparation of microcapsules containing collagen - using tranexamic acid and sodium hydroxide
[0064] (1) Add 0.2 g acetic acid to 60 g water, add 1 g chitosan until completely dissolved, then dissolve 0.2 g Tween-80, 0.2 g Span-80, and 1 g calcium chloride and homogenize until no obvious particles are formed to form solution A;
[0065] (2) Dissolve 1 g of collagen and 0.7 g of tranexamic acid in 20 g of water and mix with an appropriate amount of sodium hydroxide to uniformly disperse them in the water to form solution B;
[0066] (3) Pre-dissolve 2 g of sodium alginate in 20 g of water until it is completely dissolved to form solution C;
[0067] (4) Solution B and Solution C were added dropwise to Solution A at a dropping speed of 0.05 g / s while being homogenized at a speed of 8000 rpm to form Solution D, i.e., a microcapsule solution containing collagen.
[0068] The pH value of the microcapsule solution containing collagen was 7.3, and the Zeta potential value was -13.26 mV. It was observed that the microcapsule solution sample was obviously flocculated.
[0069] Comparative Example 3: Preparation of microcapsules containing collagen - addition of collagen
[0070] (1) Add 0.2 g acetic acid to 80 g water, add 1 g chitosan until completely dissolved, then dissolve 0.2 g Tween-80, 0.2 g Span-80, 1 g calcium chloride, 1 g collagen, and 0.7 g tranexamic acid and homogenize until no obvious particles are formed to form solution A;
[0071] (2) Pre-dissolve 2 g of sodium alginate in 20 g of water until it is completely dissolved to form solution B;
[0072] (3) Solution B was added dropwise to solution A at a dropping speed of 0.05 g / s, and homogenization was performed while the solution was added dropwise at a homogenization speed of 8000 rpm to form solution C, i.e., a microcapsule solution containing collagen.
[0073] The microcapsule samples were obviously flocculated and the microcapsules were obviously adhered.
[0074] Comparative Example 4: Preparation of microcapsules containing collagen - different dropwise addition order
[0075] (1) Dissolve 2 g of sodium alginate in 60 g of water until it is completely dissolved, then dissolve 0.2 g of Tween-80 and 0.2 g of Span-80 and mix well to form solution A.
[0076] (2) Dissolve 1 g of collagen in 20 g of water, and then disperse 0.7 g of tranexamic acid in the water to form solution B;
[0077] (3) 0.2 g acetic acid, 1 g chitosan was added to 20 g water until completely dissolved, and then 1 g calcium chloride was added until completely dissolved to form solution C;
[0078] (4) Solution B and Solution C were added dropwise to Solution A at a dropping speed of 0.05 g / s while being homogenized at a speed of 8000 rpm to form Solution D, i.e., a microcapsule solution containing collagen.
[0079] The microcapsule samples were obviously flocculated and the microcapsules were obviously adhered.
[0080] Comparative Example 5: Preparation of microcapsules containing collagen - different dropwise addition order
[0081] (1) Dissolve 2 g of sodium alginate in 60 g of water until it is completely dissolved, then dissolve 0.2 g of Tween-80 and 0.2 g of Span-80 and mix well to form solution A.
[0082] (2) Dissolve 1 g of collagen in 20 g of water, and then disperse 0.7 g of tranexamic acid in the water to form solution B;
[0083] (3) Add 1 g of chitosan to 0.2 g of acetic acid in 10 g of water until it is completely dissolved to form solution C;
[0084] (4) Add solution B and solution C to solution A at a dropping speed of 0.05 g / s while homogenizing at a speed of 8000 rpm to form solution D;
[0085] (5) Add 1 g of calcium chloride to 10 g of water until it is completely dissolved to form solution E;
[0086] (6) Solution E was added dropwise to solution D at a dropping speed of 0.05 g / s while homogenizing at a homogenizing speed of 8000 rpm to form solution F, i.e., a microcapsule solution containing collagen.
[0087] The microcapsule samples were obviously flocculated and the microcapsules were obviously adhered.
[0088] Comparative Example 6: Preparation of microcapsules containing collagen - different dropwise addition order
[0089] (1) Dissolve 2 g of sodium alginate in 60 g of water until it is completely dissolved, then dissolve 0.2 g of Tween-80 and 0.2 g of Span-80 and mix well to form solution A.
[0090] (2) Dissolve 1 g of collagen in 20 g of water, and then disperse 0.7 g of tranexamic acid in the water to form solution B;
[0091] (3) 1 g of calcium chloride is completely dissolved in 10 g of water to form solution C;
[0092] (4) Add solution B and solution C to solution A at a dropping speed of 0.05 g / s while homogenizing at a speed of 8000 rpm to form solution D;
[0093] (5) Add 1 g of chitosan to 0.2 g of acetic acid in 10 g of water until it is completely dissolved to form solution E;
[0094] (6) Solution E was added dropwise to solution D at a dropping speed of 0.05 g / s while homogenizing at a homogenizing speed of 8000 rpm to form solution F, i.e., a microcapsule solution containing collagen.
[0095] The microcapsule samples were obviously flocculated and the microcapsules were obviously adhered.
[0096] The sample photos of the microcapsules containing collagen prepared by the methods of Example 1 and Comparative Examples 1-6 are as follows: Figure 3 shown.
[0097] Example 2: Preparation of the collagen-containing microcapsule emulsion of the present invention
[0098] (1) Take 90 g of the collagen-containing microcapsule solution prepared in Example 1, and pre-dissolve 1 g of glycerol, 1 g of butanediol, and 3 g of pentanediol until they are completely dissolved to form solution A;
[0099] (2) dissolving 1 g of cetearyl glucoside in 4 g of caprylic / capric triglyceride and dispersing the mixture evenly at 80° C. to form solution B;
[0100] (3) Solution B was added to solution A and homogenized at a homogenization speed of 8000 rpm to form an emulsion sample, i.e., a microcapsule emulsion containing collagen.
[0101] The performance test results of the emulsion sample obtained in Example 2 are shown in Table 1 below.
[0102] Table 1: Performance test results of collagen microcapsule emulsion samples
[0103]
[0104]
[0105] It can be seen from the data in the above table that the collagen microcapsule emulsion sample prepared in Example 2 has a uniform and stable appearance and remains stable under high and low temperature conditions without any stratification, demulsification, etc.; the pH value is weakly acidic, which meets the relevant standards of the cosmetics industry.
[0106] Example 3: Comparison of transdermal absorption between the microcapsule emulsion containing collagen of the present invention and conventional emulsion
[0107] Referring to the preparation process of the collagen microcapsule emulsion in Example 2, a common emulsion was prepared.
[0108] The general emulsion preparation process is as follows:
[0109] (1) Take 90 g of an aqueous solution containing 0.9 g of collagen, and pre-dissolve 1 g of glycerol, 1 g of butylene glycol, and 3 g of pentanediol until they are completely dissolved to form solution A;
[0110] (2) dissolving 1 g of cetearyl glucoside in 4 g of caprylic / capric triglyceride and dispersing the mixture evenly at 80° C. to form solution B;
[0111] (3) Solution B was added to solution A and homogenized at a speed of 8000 rpm to form an emulsion sample, i.e., a common emulsion containing collagen.
[0112] The artificial membrane was directly fixed between the sample pool and the receiving pool. The sample pools were the emulsion prepared in Example 2 (sample one) and the ordinary emulsion sample (sample two), and normal saline was used as a blank control. The receiving pool was filled with normal saline to a capacity of 8 mL, and constant stirring and constant temperature were maintained. The water temperature was maintained at 37°C ± 0.5°C and the rotation speed was 200 rpm. 1 mL of samples were taken at 2, 4, 6, 8 and 24 h, and an equal amount of normal saline was added at the same time. The mass concentration of hydroxyproline in the extracted liquid was determined, and the cumulative permeation per unit area (Q n ), the concentration of hydroxyproline added to the sample pool is recorded as (Q m ), the hydroxyproline permeability is (P).
[0113]
[0114] Where: C n - Hydroxyproline mass concentration measured at the nth sampling point, μg / mL;
[0115] C i - The mass concentration of hydroxyproline measured at the i-th sampling point, μg / mL;
[0116] Conversion coefficient of 10-hydroxyproline and collagen peptide;
[0117] V-receiving pool capacity is 8mL;
[0118] V0 - 1 mL of volume is taken at each time point;
[0119] A- penetration area is 1.5cm 2 .
[0120] Determination of hydroxyproline content: GB / T9695.23-2008.
[0121] Prepare hydroxyproline standard solution: accurately weigh 50 mg of hydroxyproline, dilute to 100 mL with water, and add one drop of 3 mol / L sulfuric acid solution to make a standard solution.
[0122] Prepare a buffer solution with a pH value of 6.8 by adding 14 g of sodium hydroxide, 78 g of anhydrous acetic acid solution, 26 g of citric acid monohydrate and 250 mL of n-propanol into a 1 L volumetric flask, shake well and adjust to volume.
[0123] Prepare chloramine T solution: dissolve 1.41 g chloramine T in 100 mL of pH 6.8 buffer prepared in the previous step.
[0124] Prepare the developer solution: weigh 10 g of p-dimethylaminobenzaldehyde, dissolve it in 35 mL of 60% perchloric acid solution, mix well, slowly add 65 mL of isopropanol solution, and dilute to 100 mL in a volumetric flask.
[0125] Draw a hydroxyproline standard curve: dilute the above hydroxyproline standard solution to 0.5μg / mL, 1.0μg / mL, 1.5μg / mL, 2.0μg / mL, and 2.5μg / mL, and use deionized water as a blank sample. Take 4mL of the dilution, add 2mL of chloramine T and mix evenly, let it stand for 20 minutes in a room, then add 2mL of color developer, place it in a colorimetric tube, heat it in a 60℃ water bath for 20 minutes, take it out and cool it under running water for at least 3 minutes, let it stand for 30 minutes in a room, and then measure the absorbance value at a wavelength of 558nm±2nm.
[0126] Sample determination: After taking out the sample from the receiving pool and diluting it, add 2mL of chloramine T and mix it. After standing at room temperature for 20 minutes, add 2mL of color developer and place it in a colorimetric tube. Heat it in a 60℃ water bath for 20 minutes. After taking it out, cool it under running water for at least 3 minutes. After standing at room temperature for 30 minutes, measure the absorbance value at a wavelength of 558±2nm.
[0127] Conclusion: If Figure 2 As shown, the permeability of collagen microcapsule emulsion is significantly better than that of ordinary emulsion. It can be seen that collagen microcapsules can significantly improve the permeation and absorption efficiency of collagen, and the trend of permeation data shows that the sustained release of collagen is achieved.
[0128] Example 4: Whitening efficacy experiment
[0129] Referring to the preparation process of collagen microcapsule emulsion in Example 2, a common emulsion (sample 3) was prepared. The preparation process of sample 3 common emulsion is as follows:
[0130] (1) Take 90 g of an aqueous solution containing 0.7 g of tranexamic acid, and pre-dissolve 1 g of glycerol, 1 g of butanediol, and 3 g of pentanediol until they are completely dissolved to form solution A;
[0131] (2) dissolving 1 g of cetearyl glucoside in 4 g of caprylic / capric triglyceride and dispersing the mixture evenly at 80° C. to form solution B;
[0132] (3) Solution B was added to solution A and homogenized at a homogenization speed of 8000 rpm to form an emulsion sample, i.e., a common emulsion containing tranexamic acid.
[0133] Experimental principle: Tyrosinase can catalyze the substrate tyrosine to generate dopaquinone, and then a series of reactions will eventually generate melanin. The tyrosinase catalytic reaction is considered to be the rate-limiting step in the production of melanin, so substances that inhibit the activity of tyrosinase are considered to have potential whitening activity. Dopaquinone is a colored substance with a characteristic absorption peak at 470nm. The amount of dopaquinone generated is proportional to the activity of the enzyme. Therefore, the amount of dopaquinone generated in the system can be measured by a spectrophotometer to reflect the size of the enzyme activity.
[0134] Main reagents: tyrosinase (from mushrooms) (Shanghai Yihe Biotechnology Co., Ltd., ≥500U / mg); L-tyrosine (Aladdin, 99.0%-101.0%); α-arbutin (DSM, ≥98%); disodium hydrogen phosphate (Na2HPO4·12H2O) and sodium dihydrogen phosphate (NaH2PO4·2H2O) are all domestically produced analytical grade.
[0135] Sample preparation: The sample was diluted 8 times with phosphate buffer to obtain the test sample, and the positive control was vitamin C.
[0136] Table 2: Tyrosinase inhibition rate of microcapsule emulsion containing collagen (sample 1), common emulsion containing collagen (sample 2), and common emulsion containing tranexamic acid (sample 3)
[0137] Sample No. Sample 1 Sample 2 Sample 3 Positive Control Inhibition rate 84.21% 30.36% 52.16% 65.32%
[0138] Conclusion: As shown in Table 2, through the tyrosinase activity inhibition experiment, it was found that collagen itself has the ability to inhibit the activity of tyrosinase, but the inhibition ability is not strong. When collagen is combined with tranexamic acid, it can play a synergistic role and significantly improve the activity of tyrosinase inhibition.
[0139] Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include these modifications and variations.
Claims
1. A method for preparing microcapsules containing collagen, characterized in that: The preparation method comprises the following steps: (1) Add 0.01-1 g acetic acid or formic acid to 10-100 g water, add 0.1-5 g chitosan until it is completely dissolved, then dissolve 0.02-2 g surfactant and 0.1-5 g calcium chloride, and homogenize until no obvious particles are formed to form solution A; (2) Dissolve 0.1-5 g collagen and 0.1-1 g tranexamic acid in 5-50 g water and disperse them evenly in the water to form solution B; (3) Pre-dissolve 2 g of sodium alginate in 5-50 g of water until it is completely dissolved to form solution C; (4) Add solution B and solution C to solution A at a dropping speed of 0.01-0.1 g / s at the same time, homogenizing at a speed of 5000-10000 rpm, to form solution D, i.e., a microcapsule solution containing collagen.
2. The preparation method according to claim 1, characterized in that: The preparation method comprises the following steps: (1) Add 0.1-0.5 g acetic acid or formic acid to 30-80 g water, add 0.5-2 g chitosan until completely dissolved, then dissolve 0.2-1 g surfactant and 0.5-2 g calcium chloride, and homogenize until no obvious particles are formed to form solution A; (2) Dissolve 0.5-2g collagen and 0.5-1g tranexamic acid in 10-30g water. It is uniformly dispersed in water to form solution B; (3) Pre-dissolve 2 g of sodium alginate in 10-30 g of water until it is completely dissolved to form solution C; (4) Add solution B and solution C to solution A at a dropping speed of 0.02-0.08 g / s while homogenizing at a speed of 7000-10000 rpm to form solution D, i.e., a microcapsule solution containing collagen.
3. The preparation method according to claim 1 or claim 2, characterized in that: The surfactant is selected from one or more of the following: Tween-80, Span-80, monoglyceride of fatty acid or sucrose ester of fatty acid.
4. Microcapsules containing collagen prepared by the preparation method according to any one of claims 1 to 3.
5. A method for preparing a microcapsule emulsion containing collagen, characterized in that: The preparation method comprises the following steps: (1) taking 50-150 g of the collagen microcapsule solution of claim 4, pre-dissolving 0.1-5 g of glycerol and 0.1-15 g of polyol until they are completely dissolved to form solution A; (2) dissolving 0.1-5 g of cetearyl glucoside or glyceryl stearate in 1-10 g of fat and uniformly dispersing at 70-90° C. to form solution B; (3) Add solution B to solution A and homogenize at a speed of 5000-10000 rpm to form an emulsion sample, i.e., a microcapsule emulsion containing collagen.
6. The preparation method according to claim 5, characterized in that: The preparation method comprises the following steps: (1) taking 80-120 g of the collagen microcapsule solution of claim 4, pre-dissolving 0.5-2 g of glycerol and 0.5-10 g of polyol until they are completely dissolved to form solution A; (2) dissolving 0.5-2 g of cetearyl glucoside or glyceryl stearate in 1-10 g of caprylic capric triglyceride or jojoba oil, and dispersing the mixture evenly at 80° C. to form solution B; (3) Add solution B to solution A and homogenize at a speed of 7000-10000 rpm to form an emulsion sample, i.e., a microcapsule emulsion containing collagen.
7. The preparation method according to claim 5 or claim 6, characterized in that: In step (1), the polyol is selected from one or more of the following: propylene glycol, butylene glycol or pentylene glycol.
8. A microcapsule emulsion containing collagen prepared by the preparation method according to any one of claims 5 to 7.
9. Use of the microcapsule containing collagen according to claim 4 or the microcapsule emulsion containing collagen according to claim 8 in the preparation of cosmetics.
10. The use according to claim 9, characterized in that: The cosmetics are toner, lotion, essence, cream, ointment, facial mask or freeze-dried powder.
Citation Information
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