Emulsifier-free liquid crystal collagen peptide emulsion and preparation method thereof

By performing Maillard reaction and saponification in the emulsion, the hydrophobicity and oil stability of collagen peptides are improved, and liquid crystal collagen peptide emulsion without emulsifiers is prepared, which solves the irritation and allergic problems caused by emulsifiers, and Improves the stability and liquid crystal structure of the emulsion.

CN119280096AActive Publication Date: 2025-01-10BEIJING QINGYAN BOSHI HEALTH MANAGEMENT CO LTD
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Patent Information

Application Number
CN202411430830.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-14
Publication Date
2025-01-10
Estimated Expiration
2044-10-14

AI Technical Summary

Technical Problem

In emulsions containing collagen peptides, the addition of emulsifiers can easily lead to irritation and allergic reactions, and the high amount of collagen peptides will affect the stability of the emulsion.

Method used

By performing Maillard reaction and saponification reaction in the emulsion, glucose and xanthan gum improve the hydrophobicity of collagen peptides, and adjust the pH value through sodium hydroxide to enhance the emulsification and stability of the oil, and prepare an emulsifier-free emulsifier without emulsifiers. liquid crystal collagen peptide emulsion.

Benefits of technology

A stable collagen peptide emulsion preparation was achieved, which avoided stimulation and allergic reactions caused by emulsifiers, and significantly improved the stability of the emulsion and the formation of liquid crystal structure. A significant liquid crystal phenomenon was observed under a microscope.

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Abstract

The invention belongs to the technical field of biology, and particularly relates to a liquid crystal collagen peptide emulsion free of an emulsifier and a preparation method of the liquid crystal collagen peptide emulsion. According to the invention, glucose, xanthan gum and collagen peptide are subjected to Maillard reaction, so that the hydrophobicity of the collagen peptide is improved, and the emulsification effect on grease is realized; maillard reaction is utilized to improve the emulsifying property of the collagen peptide. The pH value is adjusted through sodium hydroxide, the Maillard reaction rate is increased, and meanwhile the stability of grease in a system is enhanced through the saponification reaction of sodium hydroxide and grease; and the emulsification effect of the grease in the system is enhanced by saponification reaction. The Maillard reaction and the saponification reaction are carried out in a water-free system, then the mixture is dropwise added into an aqueous solution, the prepared emulsion has an obvious liquid crystal state under a polarized light microscope, and the stability of the emulsion is superior to that of a common emulsion.
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Description

Technical Field

[0001] The invention belongs to the field of biotechnology, and specifically relates to an emulsifier-free liquid crystal collagen peptide emulsion and a preparation method thereof. Background Art

[0002] Collagen peptides are a series of small molecule peptides obtained by protease hydrolysis of collagen. They have small molecular weight, are easily absorbed, have multiple physiologically active functions, and have shown good application prospects in the fields of food and health care products. Collagen peptides can be used in cosmetics to play multiple roles, such as locking in moisture, anti-wrinkle and anti-aging, smoothing wrinkles, lightening and removing spots, whitening and beautifying the skin, repairing dark circles, and other multiple skin care effects.

[0003] In the preparation process of ordinary emulsions containing collagen peptides, since collagen peptides have a dual charge, when added in large amounts, it is easy to cause the thickening substances and emulsifiers in the emulsion system to become inactivated. In order to ensure the stability of 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, which is widely used in the food industry. During the reaction, amino groups and carbonyl groups undergo a variety of polymerization and condensation reactions under high temperature or heating conditions. In the multiple reaction process, studies have shown that some hydrophilic groups of collagen peptides are weakened and hydrophobic groups are strengthened, thereby improving the emulsification properties of the collagen peptides themselves.

[0005] Liquid crystal is a substance between liquid and crystal. It has both the fluidity of liquid and the anisotropy of crystal, and exhibits birefringence. In the field of cosmetics, the liquid crystal formed in the water-in-oil emulsion system is generally a lamellar liquid crystal structure. Compared with the ordinary water-in-oil emulsion system, liquid crystal cosmetics have a multi-layer liquid crystal structure at the water-oil interface. Each layer of the structure contains a large amount of bound water. During the application process, the multi-layer water is slowly released, showing an obvious long-term water-locking function. At the same time, the water-soluble functional ingredients can also achieve the purpose of sustained release. Ordinary emulsion water-in-oil systems may experience demulsification and water-oil stratification in severe environments of high and low temperatures. However, due to the multi-layer regularly arranged liquid crystal structure, liquid crystal structure emulsions still have self-recovery capabilities even after experiencing damage such as high and low temperatures, and exhibit excellent stability.

[0006] Due to the excellent water-locking and sustained-release characteristics of liquid crystal cosmetics, they are mostly used to develop functional lotions and creams. Compared with ordinary lotions and creams, liquid crystals are more conducive to the moisturizing and hydrating ingredients in the preparations, achieving twice the result with half the effort. At the same time, the sustained-release effect of the functional ingredients significantly improves the utilization rate of the functional ingredients and is more conducive to the performance of the functional ingredients. At the same time, the liquid crystal structure can reduce the use of emulsifiers in the preparations, effectively avoiding possible irritation and allergic reactions.

[0007] Inspired by the Maillard reaction principle and the working principle of liquid crystal, the inventors have discovered a method to enhance the emulsification performance of collagen peptides to replace conventional cosmetic emulsifiers, thereby reducing possible irritation and allergies in cosmetics. Summary of the invention

[0008] The present invention aims at the defects and shortcomings in the prior art and provides a liquid crystal collagen peptide emulsion without emulsifier and a preparation method thereof. The present invention prepares a collagen peptide emulsion without emulsifier through an innovative process, avoiding the irritation, allergy and other symptoms caused by the addition of emulsifiers in ordinary emulsions, and the emulsion prepared by the method of the present invention has good stability, and obvious liquid crystal formation is observed under a polarized light microscope, thereby realizing the innovative application of cosmetics containing collagen peptides.

[0009] The purpose of the present invention can be achieved through the following technical solutions:

[0010] In a first aspect, the present invention provides a method for preparing an emulsifier-free liquid crystal collagen peptide emulsion, wherein the emulsion is composed of a mixture of a phase A raw material, a phase B raw material, a phase C raw material, a phase D raw material and a phase F raw material, wherein the phase A, phase B raw material, phase C raw material, phase D raw material and phase F raw material are proportioned by weight according to the following components:

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

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

[0013] (3) Phase C: 1-10 parts of caprylic capric triglyceride;

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

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

[0016] The preparation method of the collagen peptide emulsion comprises the following steps: respectively adding the B-phase raw material and the C-phase raw material to the A-phase raw material, placing the raw material in a water bath at 70-90°C and stirring for 0.5-2h to form a composition E; heating the water to 70-90°C, adding the D-phase raw material to the water for homogenization and stirring until the D-phase raw material is fully dissolved; dropping the composition E into the D-phase aqueous solution, homogenizing while dropping, the dropping speed is 0.05g / s, and the homogenization speed is 5000-8000rpm. After dropping and homogenizing until all the raw materials are dissolved, the F-phase raw material is added to adjust the pH value of the emulsion to 6.0-7.5 to prepare the collagen peptide emulsion.

[0017] As an optional manner, in the above preparation method, the emulsion is composed of a mixture of a phase A raw material, a phase B raw material, a phase C raw material, a phase D raw material and a phase F raw material, and the phase A, phase B raw material, phase C raw material, phase D raw material and phase F raw material are proportioned by weight according to the following components;

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

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

[0020] (3) Phase C: 2-5 parts of caprylic-capric triglyceride;

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

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

[0023] The preparation method of the collagen peptide emulsion comprises the following steps: respectively adding the B-phase raw material and the C-phase raw material to the A-phase raw material, placing the raw material in a water bath at 80°C and stirring for 1h to form a composition E; heating the water to 75-80°C, adding the D-phase raw material to the water and stirring homogenously until the D-phase raw material is fully dissolved; and dropping the composition E into the D-phase aqueous solution while homogenizing, with a dropping speed of 0.05g / s and a homogenizing speed of 6000rpm. After dropping and homogenizing until all raw materials are dissolved, the F-phase raw material is added to adjust the pH value of the emulsion to 6.5-7.0 to prepare the collagen peptide emulsion.

[0024] As an optional manner, in the above preparation method, the emulsion is composed of a mixture of a phase A raw material, a phase B raw material, a phase C raw material, a phase D raw material and a phase F raw material, and the phase A, phase B raw material, phase C raw material, phase D raw material and phase F raw material are proportioned by weight according to the following components;

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

[0026] (2) Phase B: 0.2 parts of xanthan gum, 0.5 parts of glucose, 1 part of collagen peptide, and 0.1 parts of 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 comprises the following steps: respectively adding the B-phase raw material and the C-phase raw material to the A-phase raw material, placing the raw material in a water bath at 80°C and stirring for 1h to form a composition E; heating the water to 75-80°C, adding the D-phase raw material to the water and stirring homogenously until the D-phase raw material is fully dissolved; and dropping the composition E into the D-phase aqueous solution while homogenizing, with a dropping speed of 0.05g / s and a homogenizing speed of 6000rpm. After dropping and homogenizing until all raw materials are dissolved, the F-phase raw material is added to adjust the pH value of the emulsion to 6.5-7 to prepare the collagen peptide emulsion.

[0031] As an optional manner, in the above preparation method, the collagen peptide is derived from fish skin and has a molecular weight of less than 1000Da.

[0032] As an optional manner, in the above preparation method, glucose and xanthan gum undergo Maillard reaction with collagen peptides, thereby improving the hydrophobicity of the collagen peptides themselves and achieving an emulsification effect on oils and fats.

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

[0034] As an optional manner, in the above preparation method, the saponification reaction of sodium hydroxide and oil is utilized to enhance the stability of the oil in the system.

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

[0036] As an optional manner, in the above-mentioned collagen peptide emulsion, the collagen peptide emulsion has an obvious liquid crystal state under a polarized light microscope and has better stability than ordinary emulsion.

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

[0038] (1) The present invention achieves the successful preparation of a relatively stable collagen peptide emulsion without adding an emulsifier. Since collagen itself carries an electric charge, when it is added in a large amount (such as more than 1-3%) in the emulsion system, it will affect the stability of the system. The present invention solves the disadvantage of instability caused by adding a large amount of collagen. The present invention improves the hydrophobicity of the collagen peptide itself by reacting glucose and xanthan gum with the collagen peptide, and achieves an emulsification effect on oils and fats; the Maillard reaction is used to improve the emulsification performance of the collagen peptide.

[0039] (2) The present invention accelerates the Maillard reaction rate by adjusting the pH value by sodium hydroxide, and at the same time utilizes the saponification reaction of sodium hydroxide and oil to enhance the stability of the oil in the system; and utilizes the saponification reaction to enhance the emulsification effect of the oil in the system.

[0040] (3) The present invention carries out Maillard reaction and saponification reaction in a water-free system, and then adds the reaction mixture dropwise into an aqueous solution. The prepared emulsion has an obvious liquid crystal state under a polarized light microscope, and has better stability than ordinary emulsions. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 : Sample diagram of Example 1 to Example 7. In the figure, samples of Example 1 to Example 7 are shown from left to right.

[0042] Figure 2 : Liquid crystal image of the sample emulsion of Example 6. DETAILED DESCRIPTION

[0043] 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.

[0044] 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.

[0045] 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.

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

[0047] A collagen peptide emulsion, the emulsion is composed of a mixture of a phase A raw material, a phase B raw material and a phase C raw material, wherein the phase A raw material, the phase B raw material and the phase C raw material are proportioned by weight according to the following components;

[0048] (1) Phase A: 1 part glycerin, 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 of xanthan gum, 1 part of collagen peptide (derived from fish skin, molecular weight within 1000 Da, the following collagen peptide indicators are the same);

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

[0051] The preparation method of the collagen peptide emulsion comprises the following steps: heating water to 75-80°C, adding a phase B raw material into the water for homogenization and stirring until the phase B raw material is fully dissolved; mixing the phase C raw material and heating it to a solution state, adding it into the phase B for homogenization, homogenizing for 3-10 minutes, slowly stirring and cooling to 40-50°C, adding the phase A raw material while stirring until all the phase A raw material is completely dissolved, continuously stirring and cooling to about 30°C, discharging the material, and preparing the collagen peptide emulsion.

[0052] The results showed that the collagen peptide emulsion sample prepared by the method of Example 1 was kept in a -15°C refrigerator for 24 hours, and after returning to room temperature, obvious yellow colloid precipitated. The analysis formula may be the precipitation of collagen peptide under low temperature conditions.

[0053] Example 2: Preparation of collagen peptide common emulsion without emulsifier

[0054] A collagen peptide emulsion, the emulsion is composed of a mixture of a phase A raw material, a phase B raw material and a phase C raw material, wherein the phase A raw material, the phase B raw material and the phase C raw material are proportioned by weight according to the following components:

[0055] (1) Phase A: 1 part glycerin, 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, 1 part collagen peptide;

[0057] (3) Phase C: 3 parts of caprylic / capric triglyceride.

[0058] The preparation method of the collagen peptide emulsion comprises the following steps: heating water to 75-80°C, adding a phase B raw material into the water for homogenization and stirring until the phase B raw material is fully dissolved; adding a phase C raw material into the phase B for homogenization, and after homogenization for 3-10 minutes, slowly stirring and cooling to 40-50°C, adding a phase A raw material while stirring until all the phase A raw material is completely dissolved, and continuously stirring and cooling to about 30°C before discharging the material to prepare the collagen peptide emulsion.

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

[0060] Example 3: Collagen peptide common emulsion without emulsifier prepared by improved preparation process

[0061] A collagen peptide emulsion, the emulsion is composed of a mixture of a phase A raw material, a phase B raw material, a phase C raw material and a phase D raw material, wherein the phase A raw material, the phase B raw material, the phase C raw material and the phase D raw material are proportioned by weight according to the following components:

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

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

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

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

[0066] The preparation method of the collagen peptide emulsion comprises the following steps: respectively adding the raw materials of phase B and phase C to the raw materials of phase A, placing the raw materials in a water bath at 80°C and stirring for 1h to form a composition E; heating the water to 75-80°C, adding the raw materials of phase D to the water and stirring homogenously until the raw materials of phase D are fully dissolved; and dropping the composition E into the aqueous solution of phase D while homogenizing, with a dropping speed of 0.05g / s and a homogenizing speed of 6000rpm. After dropping and homogenizing, all the raw materials are dissolved to prepare the collagen peptide emulsion.

[0067] The results showed that in composition E, the color changed significantly after 1 hour, from white to slightly yellow. Based on the color, it was judged that the xanthan gum and collagen peptide underwent a Maillard reaction. However, since xanthan gum itself is a large molecular polysaccharide, the degree of the Maillard reaction was not complete.

[0068] The collagen peptide emulsion sample prepared by the method of Example 3 showed obvious stratification phenomenon after preparation, but compared with Example 2, this addition method played a role in enhancing the emulsification of collagen peptides by partial Maillard reaction, and a small amount of oil was 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 collagen peptide common emulsion without emulsifier by adding glucose

[0070] A collagen peptide emulsion, the emulsion is composed of a mixture of a phase A raw material, a phase B raw material, a phase C raw material and a phase D raw material, wherein the phase A raw material, the phase B raw material, the phase C raw material and the phase D raw material are proportioned by weight according to the following components:

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

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

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

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

[0075] The preparation method of the collagen peptide emulsion comprises the following steps: respectively adding the raw materials of phase B and phase C to the raw materials of phase A, placing the raw materials in a water bath at 80°C and stirring for 1h to form a composition E; heating the water to 75-80°C, adding the raw materials of phase D to the water and stirring homogenously until the raw materials of phase D are fully dissolved; and dropping the composition E into the aqueous solution of phase D while homogenizing, with a dropping speed of 0.05g / s and a homogenizing speed of 6000rpm. After dropping and homogenizing, all the raw materials are dissolved to prepare 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 judged that the xanthan gum, glucose and collagen peptides underwent a Maillard reaction. The degree of Maillard reaction was improved, but there was still an unemulsified oil layer. The sample liquid with glucose added was obviously yellowish. The reason for the analysis was that glucose, as a reducing sugar, could increase the degree of Maillard reaction with collagen peptides. The color of the emulsion obviously had the characteristic browning state of the Maillard reaction, but the oil layer still existed, indicating that the emulsification effect was not ideal.

[0077] Example 5: Comparison of adding citric acid to prepare a collagen peptide common emulsion without emulsifier

[0078] A collagen peptide emulsion, the emulsion is composed of a mixture of a phase A raw material, a phase B raw material, a phase C raw material, a phase D raw material and a phase F raw material, wherein the phase A raw material, the phase B raw material, the phase C raw material, the phase D raw material and the phase F raw material are proportioned by weight according to the following components;

[0079] (1) Phase A: 1 part glycerin, 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) Phase F: 0.1 parts of sodium hydroxide.

[0084] The preparation method of the collagen peptide emulsion comprises the following steps: respectively adding the B-phase raw material and the C-phase raw material to the A-phase raw material, placing the raw material in a water bath at 80°C and stirring for 1h to form a composition E; heating the water to 75-80°C, adding the D-phase raw material to the water and stirring homogenously until the D-phase raw material is fully dissolved; and dropping the composition E into the D-phase aqueous solution while homogenizing, with a dropping speed of 0.05g / s and a homogenizing speed of 6000rpm. After dropping and homogenizing until all raw materials are dissolved, the F-phase raw material is added to adjust the pH value of the emulsion to 6.5-7 to prepare the collagen peptide emulsion.

[0085] The results show that: this embodiment is to investigate the effect of acid environment on Maillard reaction, and the results show that there is no obvious change, and the oil-water separation is still obvious.

[0086] Example 6: Comparison of Preparation of Collagen Peptide Emulsion without Emulsifier by Adding Sodium Hydroxide

[0087] The collagen peptide emulsion of the present invention is composed of a mixture of a phase A raw material, a phase B raw material, a phase C raw material, a phase D raw material and a phase F raw material, wherein the phase A, phase B raw material, phase C raw material, phase D raw material and phase F raw material are proportioned by weight according to the following components:

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

[0089] (2) Phase B: 0.2 parts of xanthan gum, 0.5 parts of glucose, 1 part of collagen peptide, and 0.1 parts of 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) Phase F: 1 part of citric acid.

[0093] The preparation method of the collagen peptide emulsion comprises the following steps: respectively adding the B-phase raw material and the C-phase raw material to the A-phase raw material, placing the raw material in a water bath at 80°C and stirring for 1h to form a composition E; heating the water to 75-80°C, adding the D-phase raw material to the water and stirring homogenously until the D-phase raw material is fully dissolved; and dropping the composition E into the D-phase aqueous solution while homogenizing, with a dropping speed of 0.05g / s and a homogenizing speed of 6000rpm. After dropping and homogenizing until all raw materials are dissolved, the F-phase raw material is added to adjust the pH value of the emulsion to 6.5-7 to prepare the collagen peptide emulsion.

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

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

[0096] (1) Since xanthan gum itself is a macromolecular polysaccharide, the Maillard reaction with collagen peptides is 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 is one of the classic chemical modification technologies. It can change the spatial arrangement and composition of amino acid residues, expose and destroy some hydrophilic groups, thereby increasing the hydrophobicity of collagen peptides and giving them a certain emulsification function.

[0098] (3) The addition of sodium hydroxide reacts with the oil in a heated state to undergo a saponification reaction, forming higher fatty acids, which further emulsify the oil in the system, synergistically promoting the hydrophobic modification of collagen to enhance the emulsification performance, and can stably exert an emulsifying effect in a system without the addition of an emulsifier;

[0099] (4) First, the collagen peptide and the sugar substance undergo Maillard reaction in an anhydrous environment, i.e., a polyol system, which helps to improve the degree of the Maillard reaction. The reason is that the reactive groups are in more complete contact during the Maillard reaction in the polyol system. If the sugar substance and collagen are easily dissolved in an aqueous solution, the contact is incomplete and a full Maillard reaction cannot be carried out.

[0100] Example 7: Preparation of collagen peptide emulsion without emulsifier according to conventional process

[0101] A collagen peptide emulsion, the emulsion is composed of a mixture of a phase A raw material, a phase B raw material, a phase C raw material, a phase D raw material and a phase F raw material, wherein the phase A raw material, the phase B raw material, the phase C raw material, the phase D raw material and the phase F raw material are proportioned by weight according to the following components;

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

[0103] (2) Phase B: 0.2 parts of xanthan gum, 0.5 parts of glucose, 1 part of collagen peptide, and 0.1 parts of 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) Phase F: 1 part of citric acid.

[0107] The preparation method of the collagen peptide emulsion comprises the following steps: heating water to 75-80°C, adding a phase B raw material into the water for homogenization and stirring until the phase B raw material is fully dissolved; adding a phase C raw material into the phase B aqueous solution for homogenization, homogenizing for 3-10 minutes, slowly stirring and cooling to 40-50°C, adding a phase A raw material and a phase D raw material while stirring until the two phases of raw materials are completely dissolved, then adding a phase F raw material to adjust the pH value of the emulsion to 6.5-7, continuously stirring and cooling to about 30°C, and discharging the material to prepare the collagen peptide emulsion.

[0108] The results showed that the sample did not have the characteristic browning color of the Maillard reaction, and the separation of the water and oil layers was obvious, indicating that it was necessary to allow the collagen peptides and sugar substances to undergo the Maillard reaction before the emulsion was homogenized.

[0109] Example 8: Stability of the collagen peptide emulsion without emulsifier of the present invention

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

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

[0112]

[0113] It can be seen from the data in the above table that the emulsion sample prepared in Example 6 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.

[0114] Example 9: Liquid crystal effect of the collagen peptide emulsion without emulsifier of the present invention

[0115] Use a disposable rubber-tipped dropper to take a small amount of the sample of Example 6 onto a glass slide, carefully flatten the sample with a cover glass, place it under a polarizing microscope, and observe and photograph it at 400 times magnification to obtain the following: Figure 2 LCD image shown.

[0116] Table 2: Liquid crystal effect evaluation index

[0117]

[0118] like Figure 2 As shown, under a 400x microscope, it can be seen that the liquid crystal structure of the sample emulsion of Example 6 is complete and clear, and the 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 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 a liquid crystal collagen peptide emulsion without an emulsifier, characterized in that: The emulsion is composed of a mixture of a phase A raw material, a phase B raw material, a phase C raw material, a phase D raw material and a phase F raw material, wherein the phase A, phase B raw material, phase C raw material, phase D raw material and phase F raw material are proportioned by weight according to the following components: (1) Phase A: 1-5 parts of glycerin, 1-5 parts of butylene glycol, and 1-5 parts of propylene glycol; (2) Phase B: 0.1-2 parts of xanthan gum, 0.1-2 parts of glucose, 1-5 parts of collagen peptide, and 0.1-1 parts of sodium hydroxide; (3) Phase C: 1-10 parts of caprylic capric triglyceride; (4) Phase D: 1-5 parts of phenoxyethanol, 0.01-0.5 parts of EDTA-2Na, and 0.5-5 parts of panthenol; (5) Phase F: 1-5 parts of citric acid, The preparation method of the collagen peptide emulsion comprises the following steps: respectively adding the B-phase raw material and the C-phase raw material to the A-phase raw material, placing the raw material in a water bath at 70-90°C and stirring for 0.5-2h to form a composition E; heating the water to 70-90°C, adding the D-phase raw material to the water for homogenization and stirring until the D-phase raw material is fully dissolved; dropping the composition E into the D-phase aqueous solution, homogenizing while dropping, the dropping speed is 0.05g / s, and the homogenization speed is 5000-8000rpm. After dropping and homogenizing until all the raw materials are dissolved, the F-phase raw material is added to adjust the pH value of the emulsion to 6.0-7.5 to prepare the collagen peptide emulsion.

2. The preparation method according to claim 1, characterized in that: The emulsion is composed of a mixture of a phase A raw material, a phase B raw material, a phase C raw material, a phase D raw material and a phase F raw material, wherein the phase A, phase B raw material, phase C raw material, phase D raw material and phase F raw material are proportioned by weight according to the following components: (1) Phase A: 1-3 parts glycerin, 1-3 parts butylene glycol, 1-3 parts propylene glycol; (2) Phase B: 0.1-1 part of xanthan gum, 0.1-1 part of glucose, 1-3 parts of collagen peptide, and 0.1-0.5 parts of sodium hydroxide; (3) Phase C: 2-5 parts of caprylic-capric triglyceride; (4) Phase D: 1-2 parts of phenoxyethanol, 0.01-0.1 parts of EDTA-2Na, and 0.5-3 parts of panthenol; (5) Phase F: 1-2 parts of citric acid, The preparation method of the collagen peptide emulsion comprises the following steps: respectively adding the B-phase raw material and the C-phase raw material to the A-phase raw material, placing the raw material in a water bath at 80°C and stirring for 1h to form a composition E; heating the water to 75-80°C, adding the D-phase raw material to the water and stirring homogenously until the D-phase raw material is fully dissolved; and dropping the composition E into the D-phase aqueous solution while homogenizing, with a dropping speed of 0.05g / s and a homogenizing speed of 6000rpm. After dropping and homogenizing until all raw materials are dissolved, the F-phase raw material is added to adjust the pH value 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, glucose and xanthan gum undergo Maillard reaction with collagen peptide, thereby improving the hydrophobicity of the collagen peptide itself and achieving the emulsification effect on oil.

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 of sodium hydroxide and oil is utilized to enhance the stability of the oil in the system.

6. Liquid crystal collagen peptide emulsion without emulsifier prepared by the preparation method according to any one of claims 1 to 5.

7. The collagen peptide emulsion according to claim 6, characterized in that: The collagen peptide emulsion has an obvious liquid crystal state under a polarized light microscope and has better stability than ordinary emulsion.

Citation Information

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