Liquid crystal collagen peptide emulsion without emulsifier and preparation method thereof

By improving the emulsification properties of collagen peptides through Maillard reaction and liquid crystal structure, an emulsifier-free liquid crystal collagen peptide emulsion was prepared, solving the problems of emulsion instability and irritation/allergy, and achieving improved stability and efficacy.

CN119280096BActive Publication Date: 2026-05-01BEIJING QINGYAN BOSHI HEALTH MANAGEMENT CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
BEIJING QINGYAN BOSHI HEALTH MANAGEMENT CO LTD
Filing Date
2024-10-14
Publication Date
2026-05-01

AI Technical Summary

Technical Problem

Existing collagen peptide emulsions are prone to instability when added in large quantities. Increasing the use of emulsifiers can cause cosmetic irritation and allergy risks. In addition, ordinary emulsions are prone to demulsification and separation under high and low temperature environments.

Method used

The hydrophobicity of collagen peptides was improved by Maillard reaction. Collagen peptides were reacted with glucose and xanthan gum, and the pH value was adjusted and saponification was carried out with sodium hydroxide to prepare an emulsifier-free liquid crystal collagen peptide emulsion, forming a multilayer liquid crystal structure to improve stability.

Benefits of technology

It achieves stability and safety of emulsifier-free collagen peptide emulsion, has excellent water-locking and slow-release function, reduces the risk of irritation and allergies, and the liquid crystal structure has strong self-recovery ability at high and low temperatures.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present application belongs to the field of biotechnology, and particularly relates to a liquid crystal collagen peptide emulsion without emulsifier and a preparation method thereof. The present application improves the hydrophobicity of collagen peptide itself by Maillard reaction of glucose, xanthan gum and collagen peptide, and realizes the emulsification of oil and fat; the emulsification performance of collagen peptide is improved by Maillard reaction. The present application accelerates the Maillard reaction rate by adjusting the pH value with sodium hydroxide, and strengthens the stability of oil and fat in the system by saponification reaction of sodium hydroxide and oil and fat; the emulsification of oil and fat in the system is strengthened by saponification reaction. The present application carries out Maillard reaction and saponification reaction in a system without water, and then drops into an aqueous solution, so that the prepared emulsion has obvious liquid crystal under a polarizing microscope, and the stability is better than that of ordinary emulsion.
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Description

A liquid crystal collagen peptide emulsion without emulsifier and its preparation method Technical Field

[0001] This invention belongs to the field of biotechnology, specifically relating to a liquid crystal collagen peptide emulsion without emulsifiers and its preparation method. Background Technology

[0002] Collagen peptides are a series of small-molecule peptides obtained by hydrolyzing collagen with proteases. They have a small molecular weight, are easily absorbed, and possess various physiological activities, showing promising application prospects in the food and health product industries. In cosmetics, collagen peptides can exert multiple effects, such as locking in moisture, anti-wrinkle and delaying aging, smoothing wrinkles, fading spots and blemishes, whitening and brightening skin, and repairing dark circles, among other skincare benefits.

[0003] In the preparation of ordinary emulsions containing collagen peptides, because collagen peptides carry amphoteric charges, when a large amount is added, it can easily lead to the deactivation of thickening substances and emulsifiers in the emulsion system. In order to stabilize the emulsion, the amount of emulsifier added will be increased, but this will increase the risk of cosmetic irritation.

[0004] The Maillard reaction is a complex reaction between proteins and carbohydrates, widely used in the food industry. During the reaction, amino and carbonyl groups undergo various polymerization and condensation reactions under high temperature or heating conditions. Studies have shown that in this multiple reaction process, some hydrophilic groups of collagen peptides are weakened while hydrophobic groups are strengthened, thereby improving the emulsifying properties of the collagen peptides themselves.

[0005] Liquid crystals are substances that exist between liquids and crystals, exhibiting both the fluidity of liquids and the anisotropy of crystals, thus displaying birefringence. In the cosmetics industry, the liquid crystals formed in water-in-oil emulsion systems are generally layered liquid crystal structures. Compared to ordinary water-in-oil emulsion systems, liquid crystal cosmetics have a multi-layered liquid crystal structure at the water-oil interface, with each layer containing a large amount of bound water. During application, the water from these multiple layers is slowly released, exhibiting a significant long-lasting water-locking function, while water-soluble active ingredients can also achieve a sustained release. Ordinary water-in-oil emulsion systems may experience demulsification and water-oil separation under harsh high and low temperature environments. However, due to the regularly arranged multi-layered liquid crystal structure, liquid crystal emulsions retain self-recovery capabilities even after being subjected to high and low temperature damage, demonstrating excellent stability.

[0006] Due to their excellent water-locking and sustained-release properties, liquid crystal cosmetics are often used in the development of functional lotions and creams. Compared to ordinary lotions and creams, liquid crystal structures are more conducive to maximizing the effectiveness of moisturizing ingredients in the formulation, achieving twice the result with half the effort. Simultaneously, the sustained-release effect of the functional ingredients significantly improves their utilization rate and further enhances their efficacy. Furthermore, the liquid crystal structure can reduce the use of emulsifiers in the formulation, effectively avoiding potential irritation and allergic reactions.

[0007] Inspired by the Maillard reaction principle and the working principle of liquid crystals, the inventors have discovered a method to enhance the emulsification properties of collagen peptides, thereby replacing conventional cosmetic emulsifiers and reducing potential irritation and allergies in cosmetics. Summary of the Invention

[0008] This invention addresses the deficiencies and shortcomings of existing technologies by providing an emulsifier-free liquid crystal collagen peptide emulsion and its preparation method. This invention utilizes an innovative process to prepare an emulsifier-free collagen peptide emulsion, avoiding the irritation and allergic reactions caused by the addition of emulsifiers in ordinary emulsions. Furthermore, the emulsion prepared using this method exhibits good stability, and clear liquid crystal formation is observed under a polarized light microscope, enabling innovative applications in cosmetics containing collagen peptides.

[0009] The objective of this invention can be achieved through the following technical solutions:

[0010] In a first aspect, the present invention provides a method for preparing a liquid crystal collagen peptide emulsion without emulsifier, the emulsion being composed of a mixture of phase A raw material, phase B raw material, phase C raw material, phase D raw material and phase F raw material, wherein the phase A raw material, phase B raw material, phase C raw material, phase D raw material and phase F raw material are formulated in the following proportions by mass:

[0011] (1) Phase A: 1-5 parts glycerol, 1-5 parts butylene glycol, 1-5 parts propylene glycol;

[0012] (2) Phase B: 0.1-2 parts xanthan gum, 0.1-2 parts glucose, 1-5 parts collagen peptides, 0.1-1 parts sodium hydroxide;

[0013] (3) Phase C: Caprylic / Capric Triglyceride 1-10 parts;

[0014] (4) Phase D: 1-5 parts phenoxyethanol, 0.01-0.5 parts EDTA-2Na, 0.5-5 parts panthenol;

[0015] (5) Phase F: 1-5 parts citric acid

[0016] The preparation method of the collagen peptide emulsion includes the following steps: Phase B and Phase C raw materials are added to Phase A raw material, and stirred in a 70-90℃ water bath for 0.5-2 hours to form composition E; the water is heated to 70-90℃, and Phase D raw material is added to the water and homogenized until Phase D raw material is fully dissolved; composition E is added dropwise to the Phase D aqueous solution while homogenizing, with a dropping rate of 0.05 g / s and a homogenization rate of 5000-8000 rpm. After the addition is complete and homogenization is performed until all raw materials are completely dissolved, Phase F raw material is added to adjust the pH of the emulsion to 6.0-7.5 to prepare the collagen peptide emulsion.

[0017] Alternatively, in the above preparation method, the emulsion is composed of a mixture of phase A, phase B, phase C, phase D, and phase F raw materials, wherein the phase A, phase B, phase C, phase D, and phase F raw materials are formulated in the following proportions by mass:

[0018] (1) Phase A: 1-3 parts glycerol, 1-3 parts butylene glycol, 1-3 parts propylene glycol;

[0019] (2) Phase B: 0.1-1 part xanthan gum, 0.1-1 part glucose, 1-3 parts collagen peptides, 0.1-0.5 parts sodium hydroxide;

[0020] (3) Phase C: Caprylic / Capric Triglyceride 2-5 parts;

[0021] (4) Phase D: 1-2 parts phenoxyethanol, 0.01-0.1 parts EDTA-2Na, 0.5-3 parts panthenol;

[0022] (5) Phase F: 1-2 parts citric acid,

[0023] The preparation method of the collagen peptide emulsion involves adding phase B and phase C raw materials to phase A raw materials and stirring in an 80°C water bath for 1 hour to form composition E. The water is then heated to 75-80°C, and phase D raw materials are added to the water and homogenized until fully dissolved. Composition E is then added dropwise to the phase D aqueous solution while homogenizing at a dropping rate of 0.05 g / s and a homogenization rate of 6000 rpm. After the addition is complete and homogenization continues until all raw materials are dissolved, phase F raw materials are added to adjust the pH of the emulsion to 6.5-7.0, thus preparing the collagen peptide emulsion.

[0024] Alternatively, in the above preparation method, the emulsion is composed of a mixture of phase A, phase B, phase C, phase D, and phase F raw materials, wherein the phase A, phase B, phase C, phase D, and phase F raw materials are formulated in the following proportions by mass:

[0025] (1) Phase A: 1 part glycerol, 2 parts butylene glycol, 3 parts propylene glycol;

[0026] (2) Phase B: 0.2 parts xanthan gum, 0.5 parts glucose, 1 part collagen peptide, 0.1 parts sodium hydroxide;

[0027] (3) Phase C: 3 parts of caprylic / capric triglyceride;

[0028] (4) Phase D: 1 part phenoxyethanol, 0.05 part EDTA-2Na, 1 part panthenol;

[0029] (5) Phase F: 1 part citric acid,

[0030] The preparation method of the collagen peptide emulsion involves adding phase B and phase C raw materials to phase A raw materials and stirring in an 80°C water bath for 1 hour to form composition E. The water is then heated to 75-80°C, and phase D raw materials are added to the water and homogenized until fully dissolved. Composition E is then added dropwise to the phase D aqueous solution while homogenizing at a dropwise addition rate of 0.05 g / s and a homogenization rate of 6000 rpm. After the addition is complete and homogenization continues until all raw materials are dissolved, phase F raw materials are added to adjust the pH of the emulsion to 6.5-7, thus preparing the collagen peptide emulsion.

[0031] Alternatively, in the above preparation method, the collagen peptides are derived from fish skin and have a molecular weight of less than 1000 Da.

[0032] Alternatively, in the above preparation method, glucose and xanthan gum undergo a Maillard reaction with collagen peptides, which improves the hydrophobicity of the collagen peptides themselves and achieves emulsification of oils.

[0033] Alternatively, in the above preparation method, sodium hydroxide is used to adjust the pH value to accelerate the Maillard reaction rate.

[0034] Alternatively, in the above preparation method, the saponification reaction between sodium hydroxide and oils can be used to enhance the stability of the oils in the system.

[0035] In a second aspect, the present invention provides an emulsifier-free liquid crystal collagen peptide emulsion prepared by the preparation method described in the first aspect above.

[0036] Alternatively, in the above-mentioned collagen peptide emulsion, the collagen peptide emulsion exhibits a distinct liquid crystal appearance under a polarized light microscope, and its stability is superior to that of ordinary emulsions.

[0037] Compared with the prior art, the present invention has the following advantages:

[0038] (1) This invention enables the successful preparation of relatively stable collagen peptide emulsions without the addition of emulsifiers. Since collagen itself carries a charge, its addition in large quantities (e.g., 1-3% or more) can affect the stability of the emulsion system. This invention overcomes the instability caused by adding large amounts of collagen. This invention improves the hydrophobicity of collagen peptides by using a Maillard reaction between glucose and xanthan gum, thus achieving emulsification of oils; and utilizes the Maillard reaction to improve the emulsifying properties of collagen peptides.

[0039] (2) This invention accelerates the Maillard reaction rate by adjusting the pH value with sodium hydroxide, and at the same time enhances the stability of oils in the system by using the saponification reaction of sodium hydroxide with oils; and enhances the emulsification effect of oils in the system by using the saponification reaction.

[0040] (3) The present invention carries out Maillard reaction and saponification reaction in an anhydrous system, and then adds it dropwise to an aqueous solution. The prepared emulsion has obvious liquid crystal appearance under polarized light microscope and its stability is better than that of ordinary emulsion. Attached Figure Description

[0041] Figure 1: Sample images of Examples 1 to 7. The samples in the figure are from left to right, representing Examples 1 to 7.

[0042] Figure 2: Liquid crystal image of the sample emulsion from Example 6. Detailed Implementation

[0043] The present invention will be further described below with reference to specific embodiments. It should be understood that the specific embodiments described herein are for illustrative purposes only and are not intended to limit the scope of the invention.

[0044] Where specific techniques or conditions are not specified in the examples, they shall be performed in accordance with the techniques or conditions described in the literature in this field, or in accordance with the product instructions. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased through legitimate channels.

[0045] Unless otherwise specified, the experimental methods used in the following embodiments are conventional methods. Unless otherwise specified, the experimental materials used in the following embodiments are commercially available products.

[0046] Example 1: Preparation of a regular emulsion containing collagen peptides

[0047] A collagen peptide emulsion, the emulsion being composed of a mixture of phase A raw material, phase B raw material and phase C raw material, wherein the phase A raw material, phase B raw material and phase C raw material are formulated in the following proportions by mass;

[0048] (1) Phase A: 1 part glycerol, 2 parts butylene glycol, 3 parts propylene glycol, 1 part phenoxyethanol, 0.05 parts EDTA-2Na, 1 part panthenol;

[0049] (2) Phase B: 0.2 parts xanthan gum and 1 part collagen peptide (from fish skin, with a molecular weight of less than 1000 Da; the collagen peptide indicators are the same below).

[0050] (3) Phase C: 3 parts of caprylic acid and capric acid triglycerides, 1 part of cetyl glucoside.

[0051] The method for preparing the collagen peptide emulsion involves heating water to 75-80°C, adding phase B raw material to the water and homogenizing and stirring until phase B raw material is fully dissolved; mixing phase C raw material and heating it to a solution state, adding it to phase B and homogenizing; after homogenizing for 3-10 minutes, slowly stirring and cooling to 40-50°C; while stirring, adding phase A raw material until phase A raw material is completely dissolved; continuing to stir and cooling to about 30°C to discharge the material, thus preparing the collagen peptide emulsion.

[0052] The results showed that the collagen peptide emulsion sample prepared by the method in Example 1 was kept at -15℃ for 24 hours and then returned to room temperature, after which obvious yellow colloids were precipitated. The analysis suggests that the collagen peptides may be precipitated at low temperature.

[0053] Example 2: Preparation of a regular collagen peptide emulsion without emulsifiers

[0054] A collagen peptide emulsion, the emulsion being composed of a mixture of phase A raw material, phase B raw material and phase C raw material, wherein the phase A raw material, phase B raw material and phase C raw material are formulated in the following proportions by mass;

[0055] (1) Phase A: 1 part glycerol, 2 parts butylene glycol, 3 parts propylene glycol, 1 part phenoxyethanol, 0.05 parts EDTA-2Na, 1 part panthenol;

[0056] (2) Phase B: 0.2 parts xanthan gum and 1 part collagen peptide;

[0057] (3) Phase C: 3 parts of caprylic and capric triglycerides.

[0058] The method for preparing the collagen peptide emulsion involves heating water to 75-80°C, adding phase B raw material to the water and homogenizing and stirring until phase B raw material is fully dissolved; adding phase C raw material to phase B and homogenizing for 3-10 minutes, then slowly stirring and cooling to 40-50°C; while stirring, adding phase A raw material until phase A raw material is completely dissolved; continuing to stir and cooling to about 30°C before discharging to prepare the collagen peptide emulsion.

[0059] The results showed that the collagen peptide emulsion sample prepared by the method in Example 2 showed obvious stratification immediately after preparation, in which the originally dissolved collagen peptides also precipitated out, forming an oil layer, a collagen peptide layer and a water layer.

[0060] Example 3: A collagen peptide emulsion without emulsifiers prepared by an improved preparation process

[0061] A collagen peptide emulsion, the emulsion being composed of a mixture of phase A, phase B, phase C, and phase D raw materials, wherein the phase A, phase B, phase C, and phase D raw materials are formulated in the following proportions by mass:

[0062] (1) Phase A: 1 part glycerol, 2 parts butylene glycol, 3 parts propylene glycol;

[0063] (2) Phase B: 0.2 parts xanthan gum and 1 part collagen peptide;

[0064] (3) Phase C: 3 parts of caprylic / capric triglyceride;

[0065] (4) Phase D: 1 part phenoxyethanol, 0.05 part EDTA-2Na, 1 part panthenol.

[0066] The preparation method of the collagen peptide emulsion involves adding phase B and phase C raw materials to phase A raw materials and stirring in an 80°C water bath for 1 hour to form composition E. The water is then heated to 75-80°C, and phase D raw materials are added to the water and homogenized until phase D raw materials are fully dissolved. Composition E is then added dropwise to the phase D aqueous solution while homogenizing at a dropping rate of 0.05 g / s and a homogenization rate of 6000 rpm. Homogenization continues until all raw materials are completely dissolved, thus preparing the collagen peptide emulsion.

[0067] The results showed that the color of composition E changed significantly after 1 hour, from white to slightly yellow. Based on the color, it was determined that the xanthan gum and collagen peptides underwent a Maillard reaction. However, since xanthan gum itself is a large molecule polysaccharide, the Maillard reaction was incomplete.

[0068] The collagen peptide emulsion sample prepared using the method in Example 3 showed obvious stratification immediately after preparation. However, compared with Example 2, this addition method played a role in enhancing the emulsification of collagen peptides through Maillard reaction, with a small amount of oil emulsified to present a microemulsion state, and there was still an unemulsified oil layer on the top of the emulsion.

[0069] Example 4: Preparation of a collagen peptide emulsion without emulsifier by adding glucose

[0070] A collagen peptide emulsion, the emulsion being composed of a mixture of phase A, phase B, phase C, and phase D raw materials, wherein the phase A, phase B, phase C, and phase D raw materials are formulated in the following proportions by mass:

[0071] (1) Phase A: 1 part glycerol, 2 parts butylene glycol, 3 parts propylene glycol;

[0072] (2) Phase B: 0.2 parts xanthan gum, 0.5 parts glucose, and 1 part collagen peptide;

[0073] (3) Phase C: 3 parts of caprylic / capric triglyceride;

[0074] (4) Phase D: 1 part phenoxyethanol, 0.05 part EDTA-2Na, 1 part panthenol.

[0075] The preparation method of the collagen peptide emulsion involves adding phase B and phase C raw materials to phase A raw materials and stirring in an 80°C water bath for 1 hour to form composition E. The water is then heated to 75-80°C, and phase D raw materials are added to the water and homogenized until phase D raw materials are fully dissolved. Composition E is then added dropwise to the phase D aqueous solution while homogenizing at a dropping rate of 0.05 g / s and a homogenization rate of 6000 rpm. Homogenization continues until all raw materials are completely dissolved, thus preparing the collagen peptide emulsion.

[0076] The results showed that in composition E, the color changed significantly after 1 hour, from white to dark yellow. Based on the color, it was determined that the xanthan gum, glucose, and collagen peptides underwent a Maillard reaction. The degree of the Maillard reaction was increased, but an unemulsified oil layer still existed. The sample liquid with added glucose was significantly yellowish. The reason for this is that glucose, as a reducing sugar, can increase the degree of Maillard reaction with collagen peptides. The emulsion color clearly showed the characteristic browning of the Maillard reaction, but the oil layer still existed, indicating that the emulsification effect was not ideal.

[0077] Example 5: Comparison of preparing a regular collagen peptide emulsion without emulsifier by adding citric acid

[0078] A collagen peptide emulsion, the emulsion being composed of a mixture of phase A, phase B, phase C, phase D, and phase F raw materials, wherein the phase A, phase B, phase C, phase D, and phase F raw materials are formulated in the following proportions by mass:

[0079] (1) Phase A: 1 part glycerol, 2 parts butylene glycol, 3 parts propylene glycol;

[0080] (2) Phase B: 0.2 parts xanthan gum, 0.5 parts glucose, 1 part collagen peptide, 1 part citric acid;

[0081] (3) Phase C: 3 parts of caprylic / capric triglyceride;

[0082] (4) Phase D: 1 part phenoxyethanol, 0.05 part EDTA-2Na, 1 part panthenol;

[0083] (5) F phase: 0.1 parts of sodium hydroxide.

[0084] The preparation method of the collagen peptide emulsion involves adding phase B and phase C raw materials to phase A raw materials and stirring in an 80°C water bath for 1 hour to form composition E. The water is then heated to 75-80°C, and phase D raw materials are added to the water and homogenized until fully dissolved. Composition E is then added dropwise to the phase D aqueous solution while homogenizing at a dropwise addition rate of 0.05 g / s and a homogenization rate of 6000 rpm. After the addition is complete and homogenization continues until all raw materials are dissolved, phase F raw materials are added to adjust the pH of the emulsion to 6.5-7, thus preparing the collagen peptide emulsion.

[0085] The results showed that the purpose of this embodiment was to investigate the effect of the acid environment on the Maillard reaction. The results showed no significant change, and the oil-water separation was still obvious.

[0086] Example 6: Comparative preparation of emulsifier-free collagen peptide emulsions by adding sodium hydroxide

[0087] The present invention discloses a collagen peptide emulsion, wherein the emulsion is composed of a mixture of phase A, phase B, phase C, phase D and phase F raw materials, wherein the phase A, phase B, phase C, phase D and phase F raw materials are formulated in the following proportions by mass;

[0088] (1) Phase A: 1 part glycerol, 2 parts butylene glycol, 3 parts propylene glycol;

[0089] (2) Phase B: 0.2 parts xanthan gum, 0.5 parts glucose, 1 part collagen peptide, 0.1 parts sodium hydroxide;

[0090] (3) Phase C: 3 parts of caprylic / capric triglyceride;

[0091] (4) Phase D: 1 part phenoxyethanol, 0.05 part EDTA-2Na, 1 part panthenol;

[0092] (5) F phase: 1 part citric acid.

[0093] The preparation method of the collagen peptide emulsion involves adding phase B and phase C raw materials to phase A raw materials and stirring in an 80°C water bath for 1 hour to form composition E. The water is then heated to 75-80°C, and phase D raw materials are added to the water and homogenized until fully dissolved. Composition E is then added dropwise to the phase D aqueous solution while homogenizing at a dropwise addition rate of 0.05 g / s and a homogenization rate of 6000 rpm. After the addition is complete and homogenization continues until all raw materials are dissolved, phase F raw materials are added to adjust the pH of the emulsion to 6.5-7, thus preparing the collagen peptide emulsion.

[0094] The results showed that the collagen peptide emulsion sample prepared by the method in Example 6 was uniform and stable.

[0095] Analysis of the reasons for the successful emulsion preparation:

[0096] (1) Since xanthan gum itself is a large-molecule polysaccharide and the Maillard reaction with collagen peptides is relatively difficult and insufficient, glucose is added to enhance the degree of Maillard reaction. At the same time, the addition of sodium hydroxide adjusts the pH value of the system, which plays a role in accelerating and promoting the Maillard reaction.

[0097] (2) Maillard reaction, as a classic chemical modification technique, can improve the hydrophobicity of collagen peptides by changing the spatial arrangement and composition of amino acid residues, exposing and destroying some hydrophilic groups, thereby giving them a certain emulsifying function.

[0098] (3) The addition of sodium hydroxide reacts with the oil under heating to form higher fatty acids, which further emulsifies the oil in the system and synergistically promotes the hydrophobic modification of collagen to improve the emulsification performance. It can stably play an emulsifying role in the system without the addition of emulsifier.

[0099] (4) First, let the collagen peptides and sugars undergo the Maillard reaction in an anhydrous environment, i.e., in a polyol system. This helps to increase the degree of Maillard reaction because the reaction groups are in more complete contact during the Maillard reaction in a polyol system. If the sugars and collagen are easily dissolved in an aqueous solution, the contact will be incomplete and the Maillard reaction cannot be fully carried out.

[0100] Example 7: Preparation of an emulsifier-free collagen peptide emulsion using conventional processes.

[0101] A collagen peptide emulsion, the emulsion being composed of a mixture of phase A, phase B, phase C, phase D, and phase F raw materials, wherein the phase A, phase B, phase C, phase D, and phase F raw materials are formulated in the following proportions by mass:

[0102] (1) Phase A: 1 part glycerol, 2 parts butylene glycol, 3 parts propylene glycol;

[0103] (2) Phase B: 0.2 parts xanthan gum, 0.5 parts glucose, 1 part collagen peptide, 0.1 parts sodium hydroxide;

[0104] (3) Phase C: 3 parts of caprylic / capric triglyceride;

[0105] (4) Phase D: 1 part phenoxyethanol, 0.05 part EDTA-2Na, 1 part panthenol;

[0106] (5) F phase: 1 part citric acid.

[0107] The method for preparing the collagen peptide emulsion involves heating water to 75-80℃, adding phase B raw material to the water and homogenizing and stirring until phase B raw material is fully dissolved; adding phase C raw material to the phase B aqueous solution and homogenizing for 3-10 minutes, then slowly stirring and cooling to 40-50℃; while stirring, adding phase A and phase D raw materials until both phases are completely dissolved; then adding phase F raw material to adjust the pH of the emulsion to 6.5-7; continuing to stir and cooling to about 30℃ before discharging to obtain the collagen peptide emulsion.

[0108] The results showed that the sample did not exhibit the characteristic browning color of the Maillard reaction, and the water-oil layer was clearly separated, indicating that it is necessary to allow collagen peptides and sugars to undergo the Maillard reaction before homogenization and emulsification.

[0109] Example 8: Stability of the emulsifier-free collagen peptide emulsion of the present invention

[0110] The sample images of Examples 1 to 7 are shown in Figure 1. From left to right, the samples in the figure represent Examples 1 to 7. The performance test results of the emulsion sample obtained in Example 6 are shown in Table 1 below.

[0111] Table 1: Performance test results of the collagen peptide emulsion sample without emulsifier of the present invention

[0112]

[0113] As can be seen from the data in the table above, the emulsion sample prepared in Example 6 has a uniform and stable appearance, and remains stable under high and low temperature conditions without any layering or demulsification; the pH value is weakly acidic, which meets the relevant standards of the cosmetics industry.

[0114] Example 9: Liquid crystal effect of the emulsifier-free collagen peptide emulsion of the present invention

[0115] A small amount of the sample from Example 6 was taken with a disposable dropper and placed on a glass slide. The sample was carefully flattened with a coverslip and placed under a polarizing microscope for observation and photography at 400x magnification, resulting in the liquid crystal image shown in Figure 2.

[0116] Table 2: Evaluation Indicators for Liquid Crystal Performance

[0117]

[0118] As shown in Figure 2, under a 400x microscope, the liquid crystal structure of the sample emulsion in Example 6 is complete and clear, and its size and distribution are relatively uniform; due to the liquid crystal structure, the emulsion has an excellent smooth skin feel.

[0119] Obviously, those skilled in the art can make various modifications and variations to this invention without departing from its spirit and scope. Therefore, if these modifications and variations fall within the scope of the claims of this invention and their equivalents, this invention also intends to include these modifications and variations.

Claims

1. A method for preparing a liquid crystal collagen peptide emulsion without emulsifiers, characterized in that: The emulsion is composed of a mixture of phase A, phase B, phase C, phase D and phase F raw materials. The phase A, phase B, phase C, phase D and phase F raw materials are formulated by mass ratio of the following components: (1) Phase A: 1-3 parts glycerol, 1-3 parts butanediol, 1-3 parts propylene glycol; (2) Phase B: 0.1-1 parts xanthan gum, 0.1-1 parts glucose, 1-3 parts collagen peptides, 0.1-0.5 parts sodium hydroxide; (3) Phase C: 2-5 parts caprylic / capric triglyceride; (4) Phase D: 1-2 parts phenoxyethanol, 0.01-0.1 parts EDTA-2Na, 0.5-3 parts panthenol; (5) Phase F: 1-2 parts citric acid. The preparation method of the collagen peptide emulsion includes the following steps: phase B and phase C raw materials are added to phase A raw materials respectively, and stirred in an 80°C water bath for 1 minute. h forms composition E; water is heated to 75-80℃, and D-phase raw material is added to the water and homogenized until D-phase raw material is fully dissolved; composition E is added dropwise to the D-phase aqueous solution while homogenizing, with a dropping rate of 0.05 g / s and a homogenization rate of 6000 rpm, and homogenization is carried out until all raw materials are completely dissolved. Then, F-phase raw material is added to adjust the pH of the emulsion to 6.0-7.5 to prepare the collagen peptide emulsion. In the preparation method, glucose and xanthan gum undergo Maillard reaction with collagen peptides, which improves the hydrophobicity of collagen peptides themselves and achieves emulsification of oils. The collagen peptide emulsion has obvious liquid crystal appearance under polarized light microscopy and its stability is better than that of ordinary emulsions.

2. The preparation method according to claim 1, characterized in that: The emulsion is composed of a mixture of phase A, phase B, phase C, phase D and phase F raw materials. The phase A, phase B, phase C, phase D and phase F raw materials are formulated by mass ratio of the following components: (1) Phase A: 1 part glycerol, 2 parts butanediol, 3 parts propylene glycol; (2) Phase B: 0.2 parts xanthan gum, 0.5 parts glucose, 1 part collagen peptide, 0.1 parts sodium hydroxide; (3) Phase C: 3 parts caprylic / capric triglyceride; (4) Phase D: 1 part phenoxyethanol, 0.05 parts EDTA-2Na, 1 part panthenol; (5) Phase F: 1 part citric acid. The preparation method of the collagen peptide emulsion is to add phase B and phase C raw materials to phase A raw materials respectively, and stir under 80°C water bath conditions for 1 minute. h. Form composition E; heat water to 75-80℃, add D phase raw material to water and homogenize and stir until D phase raw material is fully dissolved; add composition E dropwise to D phase aqueous solution while homogenizing, the dropwise addition rate is 0.05 g / s and the homogenization rate is 6000 rpm, and homogenize until all raw materials are completely dissolved, then add F phase raw material to adjust the pH of the emulsion to 6.5-7.0 to prepare the collagen peptide emulsion.

3. The preparation method according to claim 1, characterized in that: In the preparation method, the collagen peptides are derived from fish skin and have a molecular weight of less than 1000 Da.

4. The preparation method according to claim 1, characterized in that: In the preparation method, sodium hydroxide is used to adjust the pH value to accelerate the Maillard reaction rate.

5. The preparation method according to claim 1, characterized in that: In the preparation method, the saponification reaction between sodium hydroxide and oils is used to enhance the stability of the oils in the system.

Citation Information

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