Composition for tightening skin as well as application and preparation method thereof
Through the compositions of truffle extract, truffle extract, kirijuana extract and Chinese Ganoderma lucidum extract, combined with the fine preparation process, the problems of multi-component synergy and active ingredient stability are solved, and the efficient stability and uniformity of the skin firming composition are achieved.
Patent Information
- Application Number
- CN202510938304.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Priority Date
- 2025-04-03
- Filing Date
- 2025-07-08
- Publication Date
- 2025-08-19
AI Technical Summary
Existing skin firming compositions ignore the synergistic effects of multi-components and lack control over the stability of active ingredients, resulting in poor skin firming effect.
The compositions of truffle extract, truffle extract, chrysanthemum extract and Chinese Ganoderma lucidum extract are used to ensure the stability and uniformity of the active ingredients through a refined preparation process, including the staged treatment of the aqueous and oil phases, temperature control and real-time monitoring of the emulsification process.
Significantly improve skin firming effect, improve the retention rate of active ingredients, reduce batch quality differences, and ensure the stability and uniformity of product efficacy.
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Figure CN120501676A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of skin care products, and in particular to a skin-tightening composition and an application and preparation method thereof. Background Art
[0002] As consumers' requirements for the efficacy of skin care products continue to increase, the development of active ingredients with anti-aging and firming functions and their stabilization technology have become a hot topic in industry research. Traditional skin-firming compositions mostly use a single plant extract (such as Ganoderma lucidum polysaccharide or algae polysaccharide) as the main active ingredient. Their formula design focuses too much on increasing the concentration of a single ingredient and ignores the synergistic effect of multiple components. In addition, the preparation process also lacks control over the stability of the active ingredient.
[0003] Chinese Patent Publication No. CN110327261 B discloses a skin-firming skin care composition and its preparation method. The composition's raw materials include an emulsifier and a thornweed flower extract; the emulsifier includes stearate and stearyl alcohol emulsifiers. This indicates that the formulation of the skin-firming skin care composition and its preparation method is designed to contain only a single active ingredient, ignoring the synergistic effects of multiple components, resulting in poor skin-firming effects.
[0004] Chinese Patent Publication No.: CN114345207A discloses a vacuum emulsification and stirring device for preparing skin care products, comprising: a tank body; a vacuum pumping component connected to the tank body; a mixed flow stirring mechanism, the mixed flow stirring mechanism including a counter-stirring assembly, a central stirring assembly and an anti-settling stirring assembly; the counter-stirring assembly is arranged around the circumference of the tank body, and the counter-stirring assembly is used to push the material at the edge of the tank body to the central stirring assembly; the central stirring assembly is vertically arranged at the center of the tank body, and is used to form a horizontal vortex inside the tank body; the anti-settling stirring assembly is arranged below the central stirring assembly, and the anti-settling stirring assembly is used to continuously turn over the material accumulated at the bottom of the tank body to the stirring area of the central stirring assembly. It can be seen that the above-mentioned vacuum emulsification and stirring device for preparing skin care products only focuses on the uniformity of the emulsion in different areas in the preparation process of skin care products, and lacks control over the stability of the key active ingredients in the skin care products. Summary of the Invention
[0005] To this end, the present invention provides a skin-tightening composition and its application and preparation method, so as to overcome the problems in the prior art of neglecting the synergistic effect of multiple components and lacking control over the stability of active ingredients.
[0006] To achieve the above objectives, the present invention provides a skin-tightening composition and its application and preparation method, wherein the composition is composed of a black truffle extract, a fork-shaped algae extract, a spilionella extract and a Chinese ganoderma lucidum extract.
[0007] Furthermore, the mass ratio of the black truffle extract, the forked algae extract, the schisandra chinensis extract and the Chinese ganoderma lucidum extract is 1:1:1:1.3.
[0008] Furthermore, the skin-tightening composition is used in the preparation of essence lotion.
[0009] Furthermore, a method for preparing an essence milk comprises:
[0010] Step S1, adding the aqueous phase base material into an emulsification reactor and performing aqueous phase homogenization treatment to obtain an aqueous phase matrix;
[0011] Step S2, melting the oil phase base material to obtain an oil phase matrix, and transferring the oil phase matrix to an emulsification reactor for emulsification to obtain an emulsified matrix;
[0012] Step S3, cooling in stages and sequentially adding the primary functional components to the emulsified matrix to obtain a primary intermediate product;
[0013] Step S4, adding the secondary functional components to the primary intermediate product in sequence to obtain a secondary intermediate product;
[0014] Step S5, adding a composite bioactive component to obtain a final product;
[0015] Step S6, sterilizing and filtering the final product;
[0016] Wherein, the aqueous phase base material includes deionized water and a hydrophilic moisturizer, a thickener and an emulsion stabilizer;
[0017] The oil phase base material includes C14-22 alcohol, C12-20 alkyl glucoside, sorbitan stearate, polysorbate 60 and a high temperature resistant skin protectant;
[0018] The first functional component includes a pH regulator and red ganoderma extract;
[0019] The second functional component includes hydroxyacetophenone, 1,2-hexanediol and a skin protectant;
[0020] The composite bioactive ingredients include palmitoyl peptide skin protective agent, biological skin protective agent, fragrance, spore tuber extract, fork algae extract, schizonepeta extract and Chinese ganoderma lucidum extract.
[0021] Furthermore, the step S2 includes:
[0022] Step S21, melting C14-22 alcohol and C12-20 alkyl glucoside in an oil phase reactor at a melting temperature of 65-70° C. to obtain an initial oil phase matrix, so as to prevent the glycosidic bond breakage of the C12-20 alkyl glucoside due to local overheating when the C12-20 alkyl glucoside is mixed with other oil phase substances and heated, and to inhibit the transesterification reaction between the C14-22 alcohol and polysorbate at high temperature;
[0023] Step S22, adding sorbitan stearate, polysorbate 60 and a high temperature resistant skin protectant to the oil phase reaction kettle, and stirring with the initial oil phase matrix at a low speed, the stirring temperature is divided into three stages, to obtain an oil phase matrix, wherein,
[0024] In the first stage, the temperature was raised to 75°C at a rate of 0.5°C / min. The temperature was slowly raised to reduce the viscosity of the oil phase matrix, allowing sorbitan stearate to be evenly dispersed. At the same time, its HLB value (hydrophile-lipophile balance) transitioned from a solid state to a molten state, forming a gradient emulsion system with polysorbate-60.
[0025] The second stage is maintained at 85°C ± 1°C for 5 minutes. The high temperature is used to convert the layered structure of alkyl glucoside and C14-22 alcohol into a cubic phase, thereby improving the encapsulation efficiency.
[0026] In the third stage, the temperature is lowered to 80°C at a rate of 1°C / min. The cooling process is used to increase the viscosity of the oil phase matrix and form an interfacial film to prevent the emulsion from merging.
[0027] Step S23, transferring the oil phase matrix in the oil phase reactor to the emulsification reactor for emulsification to obtain an emulsified matrix.
[0028] Furthermore, the step S23 includes:
[0029] Step S231, transferring the oil phase matrix to the emulsification reaction kettle;
[0030] Step S232, using a fixed amount of deionized water to high-pressure rinse the oil phase reactor, and transferring the obtained mixture of the residual oil phase matrix and the fixed amount of deionized water to the emulsification reactor;
[0031] Step S233, preliminarily mixing the oil phase matrix and the water phase matrix with low-speed stirring to obtain a water-oil blend;
[0032] Step S234, measuring the viscosity of the water-oil mixture to determine the initial stirring speed of high-speed stirring and the total time of emulsification stirring;
[0033] Step S235, stirring the water-oil mixture at the initial stirring speed to emulsify, and adjusting the emulsification stirring speed based on the viscosity measurement result during the emulsification process to obtain an emulsified base;
[0034] Among them, the mass of the quantitative deionized water is calculated based on the mass of the deionized water in the aqueous phase base material and the total mass of the oil phase base material; the initial stirring speed is calculated based on the viscosity data measured by a viscosity measuring device at the viscosity characteristic height of the water-oil blend; the viscosity characteristic height is calculated from the volume of the aqueous phase matrix and the volume of the oil phase matrix; the total time of the emulsification stirring is calculated based on the initial stirring speed.
[0035] Furthermore, in step S235, during emulsification and stirring, the viscosity of the water-oil mixture is measured at the viscosity characteristic height at regular intervals, and a viscosity measurement curve is formed. Based on the stability change of the viscosity measurement data under a preset unit time length, it is determined whether the viscosity measurement result within the corresponding time length is valid. If the stability change of the viscosity measurement data under the preset unit time length meets the preset stability standard, the viscosity measurement result within the corresponding time length is determined to be valid.
[0036] Furthermore, step S3 includes:
[0037] Step S31, stirring the emulsified base at a low speed while cooling it to 70-75°C at a rate of 4°C / min;
[0038] Step S32, adding a pH regulator to the emulsification reaction kettle and stirring at a low speed for 2 minutes to uniformly mix the pH regulator with the emulsification base;
[0039] Step S33, stirring the emulsified base at a low speed while cooling the mixture at a rate of 4°C / min to 40-45°C;
[0040] Step S34, adding the Ganoderma lucidum extract to the emulsification reaction kettle and stirring at a low speed to preliminarily mix the Ganoderma lucidum extract and the emulsification base to obtain a Ganoderma lucidum blend;
[0041] Step S35, stirring the Ganoderma lucidum blend, wherein the shear force of the stirring is divided into two periods to homogenize and disperse the Ganoderma lucidum blend to obtain a primary intermediate product;
[0042] The step S35 includes:
[0043] Step S351, primary shearing stage: stirring at a speed of 1800 RPM for 1 minute to form an initial dispersion system;
[0044] Step S352, primary compensation stage: detecting the particle size distribution value of the surface of the initial dispersion system in real time, and performing compensatory stirring whenever the particle size distribution value is greater than a first threshold value, wherein the stirring time and stirring rate of the compensatory stirring are positively correlated with the difference between the particle size distribution value and the first threshold value;
[0045] Step S353, secondary shear stage: stirring at 1500 RPM for 1 minute to stabilize the dispersion system;
[0046] Step S354, secondary compensation stage: Real-time detection of the particle size distribution of the dispersed system after stabilization. Whenever the particle size distribution is greater than a second threshold, compensatory stirring is performed. The stirring time and stirring rate of the compensatory stirring are positively correlated with the difference between the particle size distribution and the second threshold.
[0047] The first threshold is greater than the second threshold.
[0048] Furthermore, the step S4 includes:
[0049] Step S41, p-hydroxyacetophenone and 1,2-hexanediol are mixed and stirred in a 50° C. water bath for 15 minutes until completely dissolved to obtain an antioxidant-moisturizing combined solvent;
[0050] Step S42, adding the antioxidant-moisturizing combined solvent to the emulsification reactor, and stirring it with the primary intermediate product at a low speed for 3 minutes;
[0051] Step S43: adding the skin protectant to the emulsification reaction kettle and stirring at a low speed for 3 minutes to obtain a secondary intermediate product.
[0052] Furthermore, the step S5 includes:
[0053] Step S51, pre-activating the palmitoyl peptide skin protective agent;
[0054] Step S52, adding the activated p-palmitoyl peptide raw material into an emulsification reactor;
[0055] Step S53, adding the biological skin protectant and fragrance into the emulsification reactor;
[0056] Step S54, adding a composition comprising a black truffle extract, a forked algae extract, a spiltia odorifera extract, and a Chinese ganoderma lucidum extract in a mass ratio of 1:1:1:1.3 to an emulsification reactor, and stirring the mixture with the secondary intermediate product at a low speed for 3 minutes to obtain a primary product;
[0057] Step S55, performing liquid online spectrum detection on the surface of the primary product;
[0058] Step S56, calculating the activity retention rate of each extract based on the characteristic peak areas of ganoderic acid A in the Chinese Ganoderma lucidum extract, melanosporone in the Tuber melanosporum extract, spilanthol in the Spinach extract, and spilanthol in the Spinach extract obtained by the online spectral detection in step S55, and determining the compensation amount of each extract according to the activity retention rate, wherein the reliability of the activity retention rate is determined based on the comparison result of the characteristic peak area of each extract with the corresponding retention rate threshold;
[0059] Step S57: adding the corresponding extract according to the calculated compensation amount of each extract, and stirring at a low speed.
[0060] Step S58, maintaining low-speed stirring, and cooling to 35-38°C at a rate of 2°C / min to obtain the final product.
[0061] The beneficial effect of the present invention is that the composition of the black truffle extract, the forked algae extract, the schisandra chinensis extract and the Chinese ganoderma lucidum extract in a mass ratio of 1:1:1:1.3 can be used as an additive to the essence milk to significantly improve the skin condition and has the effect of significantly improving the skin and tightening the skin. Moreover, the organic ratio of the four ingredients can maximize the efficacy while reducing the amount of raw materials added.
[0062] Furthermore, the preparation method of the essence milk of the present invention improves the emulsification process and compensates by detecting the content of active substances. This compensation mechanism overcomes the problem of insufficient content of active ingredients of additives caused by the loss during the preparation process in the prior art, which in turn causes the product efficacy to fail to fully exert its effect, by improving the retention rate of key active ingredients and reducing the quality difference between batches. At the same time, it effectively ensures that the content of active substances in the prepared essence milk is accurate and the ratio is reasonable.
[0063] Furthermore, the present invention obtains an initial oil phase matrix by pre-melting C14-22 alcohol and C12-20 alkyl glucoside, thereby avoiding the glycosidic bond breakage of the alkyl glucoside due to local overheating when the C12-20 alkyl glucoside is mixed with other oil phase substances and heated, and inhibiting the ester exchange reaction between the C14-22 alcohol and polysorbate at high temperature, thereby avoiding thermal degradation byproducts.
[0064] Furthermore, the present invention divides the stirring temperature of the process of preparing the oil phase matrix from the oil phase material into three stages to obtain the oil phase matrix. In the first stage, the temperature is slowly increased to reduce the viscosity of the oil phase matrix, thereby uniformly dispersing sorbitan stearate. At the same time, its HLB value (hydrophile-lipophile balance) transitions from a solid state to a molten state, thereby forming a gradient emulsification system with polysorbate 60. In the second stage, the high temperature is maintained to convert the layered structure of the alkyl glucoside and the C14-22 alcohol into a cubic phase, thereby improving the encapsulation efficiency. In the third stage, the temperature is lowered to recover the viscosity of the oil phase matrix, thereby forming an interfacial film to prevent the emulsion from merging.
[0065] Furthermore, the present invention uses a certain amount of deionized water to high-pressure flush the oil phase reactor after the oil phase matrix is transferred, thereby reducing the residual oil phase matrix and ensuring the composition ratio of the essence milk.
[0066] Furthermore, the present invention dynamically adjusts the shear force intensity during the emulsification and stirring process by real-time monitoring of the system's rheological properties, triggering negative compensation when the viscosity is less than a threshold value to prevent emulsion breakage caused by excessive shearing and enhance batch stability. At the same time, the emulsification process is precisely controlled to obtain an emulsified matrix with excellent performance, which effectively assists in the subsequent addition of functional components and bioactive components.
[0067] Furthermore, the present invention measures the particle size distribution of the Ganoderma lucidum blend and, in combination with the accumulated compensation times, performs double compensation regulation on the Ganoderma lucidum blend, thereby improving the particle size uniformity of the system and greatly improving the in vitro transdermal penetration rate of Ganoderma lucidum A.
[0068] Furthermore, the present invention pre-activates the palmitoyl peptide raw materials, wherein the guanidine group of arginine binds to the hydrophobic region of the peptide chain, destroying the intermolecular hydrogen bonds and hydrophobic forces, thereby dissociating the aggregates; thermal oscillation at 45°C causes the α-helical structure to partially unfold, exposing the active site and increasing its transdermal absorption rate; at the same time, the pre-activated palmitoyl peptide exposes the palmitic acid hydrophobic end, which self-assembles with the steroidal structure of ganoderic acid A in the Chinese Ganoderma lucidum extract through hydrophobic interaction to form a nanocomplex, which can simultaneously activate the TGF-β / Smad pathway (peptide action) and the Nrf2 antioxidant pathway (ganoderic acid action), thereby increasing the amount of collagen synthesis in fibroblasts. BRIEF DESCRIPTION OF THE DRAWINGS
[0069] Figure 1 This is a flow chart of a method for preparing an essence milk of the present invention;
[0070] Figure 2 This is a flow chart of step S2 of a method for preparing an essence milk according to the present invention;
[0071] Figure 3 This is a flow chart of step S23 of a method for preparing an essence milk according to the present invention;
[0072] Figure 4 This is a flow chart of step S3 of a method for preparing an essence milk according to the present invention;
[0073] Figure 5 This is a flow chart of step S5 of a method for preparing an essence milk according to the present invention. DETAILED DESCRIPTION
[0074] In order to make the objects and advantages of the present invention more clearly understood, the present invention is further described below in conjunction with embodiments; it should be understood that the specific embodiments described herein are merely used to explain the present invention and are not intended to limit the present invention.
[0075] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only used to explain the technical principles of the present invention and are not intended to limit the scope of protection of the present invention.
[0076] It should be noted that, in the description of the present invention, terms such as "upper", "lower", "inside" and "outside" indicating directions or positional relationships are based on the directions or positional relationships shown in the accompanying drawings. This is only for the convenience of description and does not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation. Therefore, it cannot be understood as a limitation on the present invention.
[0077] Furthermore, it should be noted that, in the description of the present invention, unless otherwise expressly specified or limited, the terms "mounted" and "connected" should be understood in a broad sense. For example, they may refer to fixed, detachable, or integral connections; mechanical or electrical connections; direct or indirect connections through an intermediate medium; or internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.
[0078] See also Figure 1 As shown in FIG, it is a flow chart of a method for preparing an essence milk of the present invention; the present invention provides a method for preparing an essence milk, comprising:
[0079] Step S1, adding the aqueous phase base material into an emulsification reactor and performing aqueous phase homogenization treatment to obtain an aqueous phase matrix;
[0080] Specifically, step S1 includes:
[0081] Step S11, adding deionized water, a hydrophilic moisturizer, a thickener, and an emulsion stabilizer to an emulsification reactor in sequence and stirring at a low speed to preliminarily mix the aqueous phase base materials to obtain an aqueous phase blend;
[0082] In one embodiment, the hydrophilic moisturizer includes sodium hyaluronate and propylene glycol, the thickener includes acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer, and the emulsion stabilizer includes ammonium acryloyldimethyltaurate / VP copolymer; the aqueous phase base material refers to a hydrophilic material, and the oil phase material refers to a lipophilic material, which is easily understood by those skilled in the art and will not be elaborated here.
[0083] Step S12, stirring the aqueous phase blend at a high speed while heating it to 80-85° C. at a rate of 2° C. / min to homogenize and disperse it to obtain an aqueous phase matrix;
[0084] It can be understood that the low-speed stirring described in this embodiment is 30RPM~40RPM according to the conventional preparation of essence milk, and the high-speed stirring described is 2000RPM~2500RPM according to the conventional preparation of essence milk. Preferably, the low-speed stirring involved in the present invention is 35RPM, and the high-speed stirring involved is 2000RPM.
[0085] Step S2: After pre-melting the oil phase base material, an oil phase matrix is obtained, and the oil phase matrix is transferred to an emulsification reactor for emulsification to obtain an emulsified matrix.
[0086] In practice, the oil phase base material includes C14-22 alcohol, C12-20 alkyl glucoside, sorbitan stearate, polysorbate 60 and a high temperature resistant skin protectant. Preferably, in this embodiment, the high temperature resistant skin protectant includes sunflower seed oil.
[0087] For more details, please refer to Figure 2 As shown, it is a flow chart of step S2 of a method for preparing an essence milk of the present invention, and the step S2 comprises:
[0088] Step S21, melting C14-22 alcohol and C12-20 alkyl glucoside in an oil phase reactor, controlling the melting temperature at 65-70° C. to obtain an initial oil phase matrix;
[0089] Step S22, adding sorbitan stearate, polysorbate-6 and a high temperature resistant skin protectant to the oil phase reaction kettle, and stirring with the initial oil phase matrix at a low speed, the stirring temperature is divided into three stages, to obtain an oil phase matrix, wherein,
[0090] In the first stage, the temperature was raised to 75°C at a rate of 0.5°C / min. The temperature was slowly raised to reduce the viscosity of the oil phase matrix, allowing sorbitan stearate to be evenly dispersed. At the same time, its HLB value (hydrophile-lipophile balance) transitioned from a solid state to a molten state, forming a gradient emulsion system with polysorbate-60.
[0091] The second stage is maintained at 85°C ± 1°C for 5 minutes. The high temperature is used to convert the layered structure of alkyl glucoside and C14-22 alcohol into a cubic phase, thereby improving the encapsulation efficiency.
[0092] In the third stage, the temperature is lowered to 80°C at a rate of 1°C / min. The cooling process is used to increase the viscosity of the oil phase matrix and form an interfacial film to prevent the emulsion from merging.
[0093] Step S23, transferring the oil phase matrix in the oil phase reactor to the emulsification reactor for emulsification to obtain an emulsified matrix.
[0094] Specifically, step S23 includes:
[0095] Step S231, transferring the oil phase matrix to the emulsification reaction kettle;
[0096] Step S232, using a fixed amount of deionized water to high-pressure rinse the oil phase reactor, and transferring the obtained mixture of the residual oil phase matrix and the fixed amount of deionized water to the emulsification reactor;
[0097] Step S233, preliminarily mixing the oil phase matrix and the water phase matrix with low-speed stirring to obtain a water-oil blend;
[0098] Step S234, measuring the viscosity of the water-oil mixture to determine the initial stirring speed of high-speed stirring and the total time of emulsification stirring;
[0099] Step S235, stirring the water-oil mixture at the initial stirring speed to emulsify, and adjusting the emulsification stirring speed based on the viscosity measurement result during the emulsification process to obtain an emulsified base;
[0100] Among them, the mass of the quantitative deionized water is calculated based on the mass of the deionized water in the aqueous phase base material and the total mass of the oil phase base material; the initial stirring speed is calculated based on the viscosity data measured by a viscosity measuring device at the viscosity characteristic height of the water-oil blend; the viscosity characteristic height is calculated from the volume of the aqueous phase matrix and the volume of the oil phase matrix; the total time of the emulsification stirring is calculated based on the initial stirring speed.
[0101] In a specific embodiment, the amount of deionized water is determined by the following formula:
[0102] Quantitative deionization = 8% × the mass of deionized water in the aqueous phase base material + 5% × the total mass of the oil phase base material
[0103] In a specific embodiment, the viscosity of the water-oil mixture is measured by an online vibrating viscosity sensor.
[0104] The characteristic viscosity height is determined by the following formula:
[0105] Calculate the ratio of the volume of the aqueous matrix to the volume of the water-oil blend, i.e., aqueous phase volume fraction = aqueous phase volume / (aqueous phase volume + oil phase volume);
[0106] Calculate the ratio of the volume of the oil phase matrix to the volume of the water-oil blend, i.e., oil phase volume fraction = oil phase volume / (water phase volume + oil phase volume);
[0107] According to the geometric parameters of the emulsification reactor, the effective mixing height is defined as 80% of the total height of the liquid level in the reactor; therefore, the calculation formula for the viscosity characteristic height is:
[0108] Viscosity characteristic height = water phase volume fraction × effective mixing height × water phase distribution weight factor + oil phase volume fraction × effective mixing height × oil phase distribution weight factor, unit is meter (m);
[0109] It can be understood that the present invention determines the minimum ratio range of the water phase distribution weight factor and the oil phase distribution weight factor according to the water-oil density ratio. Preferably, the water phase distribution weight factor is 0.7 and the oil phase distribution weight factor is 0.3.
[0110] In practice, the initial stirring speed in step S234 is determined by the following formula:
[0111] At the viscosity characteristic height, the initial intrinsic viscosity is measured using an online vibration viscosity measuring device, in cP;
[0112] According to the viscosity-speed response model, the reference speed is calculated:
[0113] Reference speed = 500 × (initial intrinsic viscosity / reference viscosity reference value) ^ 0.2;
[0114] Preferably, the reference viscosity base value is 1000, in cP;
[0115] Introduce the volume fraction correction term:
[0116] Correction coefficient = 1 + 0.2 × (oil phase volume fraction - 0.5);
[0117] It can be understood that when the volume fraction of the oil phase is greater than 50%, the correction coefficient is greater than 1, and vice versa;
[0118] Therefore, the initial stirring speed calculation formula is:
[0119] Initial stirring speed = reference speed × correction factor, the unit is revolutions per minute (PRM).
[0120] The total time of the emulsification stirring is determined by the following formula:
[0121] The total time of emulsification stirring = basic time term + speed / viscosity coupling term, in minutes (min), where:
[0122] The basic time item is It is negatively correlated with the initial stirring speed. The higher the initial stirring speed, the shorter the basic emulsification time.
[0123] The velocity / viscosity coupling term is Characterizes the matching degree between the initial stirring speed and the viscosity threshold. When the ratio is smaller, that is, high speed and low viscosity, the coupling time is shorter.
[0124] Preferably, the coefficient m1 is 4000; the coefficient m2 is 1.5; and the viscosity threshold is 2000, in cP.
[0125] Specifically, in step S235, during emulsification and stirring, the viscosity of the water-oil mixture is measured at the viscosity characteristic height at regular intervals to form a viscosity measurement curve. Based on the stability change of the viscosity measurement data under a preset unit time length, it is determined whether the viscosity measurement result within the corresponding time length is valid. If the stability change of the viscosity measurement data under the preset unit time length meets the preset stability standard, the viscosity measurement result within the corresponding time length is determined to be valid, and the viscosity measurement result determined to be valid is used as the initial characteristic viscosity for the above calculation.
[0126] It is understood that the stability change of the following viscosity measurement data can represent the uniformity of the emulsification of the water-oil blend. In the present invention, the stability change of the viscosity measurement data meeting the preset stability standard can be defined as the variance value of each viscosity measurement data not exceeding the maximum limit variance. The preset unit time period is generally 1 minute to 3 minutes. Preferably, the maximum limit variance is generally any value between 1.5 and 2.
[0127] In a specific embodiment, the viscosity of the water-oil mixture is measured at the viscosity characteristic height every 30 seconds, and the stirring rate adjustment amount is determined by the following formula:
[0128] Stirring rate adjustment amount = direction control term × dynamic adjustment term, wherein the direction control term is the sign function sgn (viscosity measurement value - viscosity threshold value). It can be understood that,
[0129] When the viscosity measurement value is greater than the viscosity threshold, take +1 (positive adjustment);
[0130] When the viscosity measurement value = viscosity threshold, it is 0 (no adjustment);
[0131] When the viscosity measurement value is less than the viscosity threshold, take -1 (negative adjustment);
[0132] The dynamic adjustment items are:
[0133] in,
[0134] It is the viscosity deviation driving term, which quantifies the relative deviation between the real-time viscosity and the threshold. The larger the deviation, the higher the adjustment intensity.
[0135] k1×current stirring time is the time cumulative effect term, which realizes the linear enhancement of stirring rate adjustment over time;
[0136] is the initial speed attenuation term, which reflects the negative correlation of the initial stirring speed. The higher the initial speed, the smaller the unit stirring rate adjustment;
[0137] Preferably, the coefficient k1 is 0.8; the coefficient k2 is 250.
[0138] The present invention uses an online vibrating viscosity sensor to monitor the rheological properties of the system in real time. First, the measurement position of the vibrating viscosity sensor is determined in combination with the ratio of the water phase to the oil phase in the matrix to ensure the representativeness of the measurement data in the system; then, the initial parameters of the emulsification process are determined, including the initial stirring speed and the total time of the emulsification stirring; finally, the shear force intensity of the emulsification stirring process is dynamically adjusted by combining the time accumulation effect and the initial speed decay algorithm, and negative compensation is triggered when the viscosity is less than a threshold value to prevent excessive shearing from causing emulsion breakage and enhance batch stability; at the same time, the emulsification process is precisely controlled to obtain an emulsified matrix with excellent performance, which can effectively assist in the subsequent addition of functional components and bioactive components. For example, when the viscosity of the emulsified matrix is relatively high, increasing the shear force intensity of the stirring can effectively break the entanglement network of the polymer and reduce the degradation rate of heat-sensitive components such as ganoderic acid A.
[0139] Step S3, cooling in stages and sequentially adding the primary functional components to the emulsified matrix to obtain a primary intermediate product;
[0140] In practice, the first functional component includes a pH regulator and Ganoderma lucidum extract.
[0141] Specifically, step S3 includes:
[0142] Step S31, stirring the emulsified base at a low speed while cooling it to 70-75°C at a rate of 4°C / min;
[0143] Step S32, adding a pH regulator to the emulsification reaction kettle and stirring at a low speed for 2 minutes to uniformly mix the pH regulator with the emulsification base;
[0144] Preferably, the pH adjuster is tetrahydroxypropylethylenediamine.
[0145] Step S33, stirring the emulsified base at a low speed while cooling the mixture at a rate of 4°C / min to 40-45°C;
[0146] Step S34, adding the Ganoderma lucidum extract to the emulsification reaction kettle and stirring at a low speed to preliminarily mix the Ganoderma lucidum extract and the emulsification base to obtain a Ganoderma lucidum blend;
[0147] Step S35, stirring the Ganoderma lucidum blend, wherein the shear force of the stirring is divided into two periods to homogenize and disperse the Ganoderma lucidum blend to obtain a primary intermediate product;
[0148] Specifically, the step S35 includes:
[0149] Step S351, primary shearing stage: stirring at a speed of 1800 RPM for 1 minute to form an initial dispersion system;
[0150] Step S352, primary compensation stage: detecting the particle size distribution of the Ganoderma lucidum blend in real time, and performing compensatory stirring whenever the particle size distribution is greater than a first threshold value, wherein the stirring time and stirring rate of the compensatory stirring are positively correlated with the difference between the particle size distribution and the first threshold value;
[0151] Step S353, secondary shear stage: stirring at 1500 RPM for 1 min to stabilize the dispersion system;
[0152] Step S354, secondary compensation stage: real-time detection of the particle size distribution of the Ganoderma lucidum blend, and whenever the particle size distribution is greater than a second threshold, compensatory stirring is performed, wherein the stirring time and stirring rate of the compensatory stirring are positively correlated with the difference between the particle size distribution and the second threshold;
[0153] The first threshold is greater than the second threshold.
[0154] In a specific embodiment, the particle size distribution of the Ganoderma lucidum blend is measured by an online laser particle size analyzer, and the particle size distribution is D 90 , that is, measuring the particle size of 90% of the cumulative distribution, the stirring time and stirring rate of the compensation stirring in the primary compensation stage and the secondary compensation stage are determined by the following formula:
[0155] In the primary compensation stage, whenever D 90 >D0, there is
[0156]
[0157] Where:
[0158] D0 is the first threshold, in micrometers (μm);
[0159] Δt1 is the primary mixing time, in seconds (s);
[0160] ΔRPM1 is the primary compensation rate in revolutions per minute (RPM);
[0161] T c The number of compensations accumulated during the primary compensation stage;
[0162] In the preparation method provided by the present invention, preferably D0=20, and the primary compensation is performed by stirring at (1800+ΔRPM1)RPM for Δt1 seconds;
[0163] Specifically, in the secondary compensation stage, whenever D 90 >D0', there is
[0164]
[0165] Where:
[0166] D0' is the second threshold, in micrometers (μm);
[0167] Δt2 is the secondary compensation time, in seconds (s);
[0168] ΔRPM2 is the secondary compensation rate in revolutions per minute (RPM);
[0169] T c ' is the cumulative number of compensations in the secondary compensation stage;
[0170] In the preparation method provided by the present invention, D0′=18, and the secondary compensation is performed by stirring at (1500+ΔRPM2)RPM for Δt2 seconds;
[0171] It can be understood that when the particle size of 90% of the measured cumulative distribution is greater than the threshold value, as the deviation between the actual particle size and the target value increases, the adjustment level of the compensating stirring is gradually increased, and the intensity of the adjustment is gradually enhanced through the accumulated number of compensations in each stage. The actual implementer can set the first threshold and the second threshold according to the actual situation or the historical data of the Ganoderma lucidum blend of the essence milk that has passed the test.
[0172] The present invention uses an online laser particle size analyzer to measure the particle size distribution of the Ganoderma lucidum blend, and combines the accumulated number of compensations to perform dual compensation regulation on the Ganoderma lucidum blend, thereby improving the particle size uniformity of the system and greatly improving the in vitro transdermal rate of Ganoderma lucidum A. The accumulated number of compensations in each stage reflects the "memory effect" of the process system, that is, if multiple compensations still fail to meet the standards, the intensity of the regulation needs to be gradually increased to cope with the aggregation of stubborn particles. At the same time, a lower limit of the compensation time is set in the secondary compensation stage (even if the calculated value is smaller, it is executed for at least 5 seconds), which takes into account the minimum processing time required for the start-stop inertia of the equipment, avoids insufficient mixing due to too small a calculated value, and ensures that small deviations close to the threshold are still effectively processed.
[0173] Step S4, adding the secondary functional components to the primary intermediate product in sequence to obtain a secondary intermediate product;
[0174] Specifically, step S4 includes:
[0175] Step S41, p-hydroxyacetophenone and 1,2-hexanediol are mixed and stirred in a 50° C. water bath for 15 minutes until completely dissolved to obtain an antioxidant-moisturizing combined solvent;
[0176] Step S42, adding the antioxidant-moisturizing combined solvent to the emulsification reactor, and stirring it with the primary intermediate product at a low speed for 3 minutes;
[0177] Step S43, adding the skin protectant to the emulsification reaction kettle and stirring at a low speed for 3 minutes to obtain a secondary intermediate product;
[0178] Preferably, the skin protective agent comprises dipotassium glycyrrhizate and hydroxypropyl tetrahydropyrantriol in sequence.
[0179] Step S5, adding a composite bioactive component to obtain a final product;
[0180] Please continue reading Figure 3 , which is a flow chart of step S5 of a method for preparing an essence milk of the present invention. Specifically, step S5 includes:
[0181] Step S51, pre-activating the palmitoyl peptide skin protective agent;
[0182] Preferably, the palmitoyl peptide skin protectant includes palmitoyl tripeptide-1, palmitoyl tetrapeptide-7 and palmitoyl pentapeptide-4.
[0183] In a specific embodiment, the pre-activation treatment of the palmitoyl peptide skin protectant is as follows: dissolving the palmitoyl peptide in a pH 6.0 buffer solution containing 0.1 mol / L arginine, shaking in a water bath at 45° C. for 30 min,
[0184] The present invention performs a pre-activation treatment on a palmitoyl peptide skin protectant, wherein the guanidine group of arginine combines with the hydrophobic region of the peptide chain, destroying the intermolecular hydrogen bonds and hydrophobic forces, thereby dissociating the aggregates; thermal oscillation at 45°C causes the α-helical structure to partially unfold, exposing the active site and increasing its transdermal absorption rate; at the same time, the palmitic acid hydrophobic end of the pre-activated palmitoyl peptide is exposed, and self-assembles with the steroid structure of ganoderic acid A in the Chinese ganoderma lucidum extract through hydrophobic interaction to form a nanocomplex. The complex can simultaneously activate the TGF-β / Smad pathway (peptide action) and the Nrf2 antioxidant pathway (ganoderic acid action), thereby increasing the amount of collagen synthesis in fibroblasts.
[0185] Step S52, adding the activated palmitoyl peptide skin protective agent into an emulsification reactor;
[0186] Step S53, adding the biological skin protectant and fragrance into the emulsification reactor;
[0187] In practice, preferably, the biological skin protectant includes isosorbide dimethyl ether, PEG / PPG-14 / 7 dimethyl ether, succinoglycan, arginine / lysine polypeptide, hybrid rose extract and gardenia fruit extract.
[0188] Preferably, the fragrance comprises daily fragrance.
[0189] Step S54, adding a composition comprising a black truffle extract, a forked algae extract, a spiltia odorifera extract, and a Chinese ganoderma lucidum extract in a mass ratio of 1:1:1:1.3 to an emulsification reactor, and stirring the mixture with the secondary intermediate product at a low speed for 3 minutes to obtain a primary product;
[0190] Step S55, performing online spectrum detection on the surface of the primary product;
[0191] Step S56, calculating the activity retention rate of each extract based on the characteristic peak areas of ganoderic acid A in the Chinese Ganoderma lucidum extract, melanosporone in the Tuber melanosporum extract, spilanthol in the Spinach extract, and spilanthol in the Spinach extract obtained by the online spectral detection in step S55, and determining the compensation amount of each extract according to the activity retention rate, wherein the reliability of the activity retention rate is determined based on the comparison result of the characteristic peak area of each extract with the corresponding retention rate threshold;
[0192] In a specific embodiment, an online NIR probe is installed on the side wall of the emulsification reactor to perform online near-infrared spectroscopy on the primary product, and the characteristic peak areas of ganoderic acid A in the Chinese Ganoderma lucidum extract, melanosporone in the black truffle extract, spilanthol in the spilanthol extract, and spilantholide in the spilanthol extract are obtained by partial least squares method, and their activity retention rates are calculated;
[0193] The reliability of each activity retention rate is determined based on the comparison result of the difference between each activity retention rate and the corresponding retention rate threshold. The reliability of the activity retention rate is determined by the following formula:
[0194] Reliability index = absolute deviation term × spectral fluctuation correction term, where
[0195] The absolute deviation term is
[0196] The spectral fluctuation correction term is
[0197] If the reliability index is ≤1, the test result is considered reliable and is used to calculate the activity retention rate;
[0198] If 1 < reliability index ≤ 2, the retest mechanism is triggered (a 5-second low-speed stirring is performed and an additional online spectrum detection is performed);
[0199] If the reliability index is greater than 2, the data is judged to be abnormal and the self-check program is started;
[0200] Preferably, each retention rate threshold is 98% or a value between 90% and 99%.
[0201] When the reliability of the activity retention rate of each extract is judged to be qualified, the representative activity retention rate is calculated, and the representative activity retention rate is determined by the following formula:
[0202] Characterization activity retention rate = (1.3 × Q1 + Q2 + Q3 + Q4) / 4.3,
[0203] Among them, Q1, Q2, Q3, and Q4 are the activity retention rates of Chinese Ganoderma lucidum extract, Black Truffle extract, Crossleaf Algae extract, and Globe Thermae extract, respectively.
[0204] The extract compensation amount is determined by the following formula:
[0205] First, calculate the total extract compensation amount,
[0206] Total extract compensation amount = s × (retention rate threshold - characterization activity retention rate) × reference total mass,
[0207] Wherein, the reference total mass = 4.3 g / kg.
[0208] Preferably, the coefficient s is 80.
[0209] The total extract compensation is split into individual extract compensations based on the original mass ratios:
[0210] The amount of black truffle extract compensation = 1 / 4.3 × total extract compensation,
[0211] The amount of the extract of the genus Alpinia serrata is compensated = 1 / 4.3 × the amount of the total extract.
[0212] Compensation amount of Spinach extract = 1 / 4.3 × total extract compensation amount,
[0213] Compensation amount of Chinese Ganoderma lucidum extract = 1.3 / 4.3 × compensation amount of total extract.
[0214] The characteristic peak base area, detection wavelength and standard deviation of each extract are shown in the following table:
[0215]
[0216] The present invention uses an online near-infrared spectrometer to detect the retention rate of active ingredients of each key extract in the initial product, and accurately compensates on demand, so that the key active ingredients still maintain a high retention rate under extreme process conditions (such as excessive shearing). In addition, by splitting the ratio, the change of each compensation amount to the component ratio of the composition is very small, thereby ensuring the product efficacy.
[0217] Step S57, adding the corresponding extract according to the calculated compensation amount of each extract, and stirring at a low speed;
[0218] Step S58, maintaining low-speed stirring, and cooling to 35-38°C at a rate of 2°C / min to obtain the final product.
[0219] Step S6: sterilize and filter the final product.
[0220] Example 1
[0221] Step S11: 60 kg of deionized water, 20 kg of propylene glycol, 0.5 kg of sodium hyaluronate, 0.5 kg of acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer, and 1 kg of ammonium acryloyldimethyltaurate / VP copolymer were sequentially added to an emulsification reactor, and stirred at 35 RPM to preliminarily mix the aqueous phase base materials to obtain an aqueous phase blend.
[0222] Step S12, stirring the aqueous phase blend at 2000 RPM while heating to 80-85° C. at a rate of 2° C. / min to homogenize and disperse the aqueous phase to obtain an aqueous phase matrix;
[0223] Step S21, melting 1 kg of C14-22 alcohol and 1 kg of C12-20 alkyl glucoside in an oil phase reactor, controlling the melting temperature at 65-70° C. to obtain an initial oil phase matrix;
[0224] Step S22, adding 2 kg of sorbitan stearate, 2 kg of polysorbate-64 kg, and sunflower seed oil to the oil phase reaction kettle, and stirring with the initial oil phase matrix at 35 RPM, with the stirring temperature divided into three stages, to obtain an oil phase matrix;
[0225] The three stages of the stirring temperature in step S22 are as follows: the first stage is to increase the temperature to 75°C at 0.5°C / min, the second stage is to maintain the temperature at 85°C±1°C for 5 minutes, and the third stage is to decrease the temperature to 80°C at 1°C / min;
[0226] Step S231, transferring the oil phase matrix to the emulsification reaction kettle;
[0227] Step S232, using 5.3 kg of deionized water to high-pressure rinse the oil phase reactor, and transferring the remaining oil phase matrix and the quantitative deionized water to the emulsification reactor;
[0228] Step S233, stirring at 35 RPM to preliminarily mix the oil phase matrix and the water phase matrix to obtain a water-oil blend;
[0229] Step S234, measuring the viscosity of the water-oil mixture to determine the initial stirring speed of high-speed stirring and the total time of emulsification stirring;
[0230] Step S235, stirring the water-oil mixture at the initial stirring speed to emulsify, and adjusting the emulsification stirring speed based on the result of viscosity measurement during the emulsification process to obtain an emulsified base;
[0231] Step S31, stirring the emulsified base at 35 RPM while cooling to 70-75°C at a rate of 4°C / min;
[0232] Step S32: add 1 kg of tetrahydroxypropylethylenediamine to the emulsification reaction kettle and stir at 35 RPM for 2 minutes to mix it with the emulsification base.
[0233] Step S33, stirring the emulsified base at 35 RPM while cooling the mixture at a rate of 4°C / min to 40-45°C;
[0234] Step S34, adding 1 kg of Ganoderma lucidum extract to the emulsification reactor, stirring at 35 RPM to preliminarily mix the Ganoderma lucidum extract and the emulsification base to obtain a Ganoderma lucidum blend;
[0235] Step S35, stirring the Ganoderma lucidum blend, wherein the shear force of the stirring is divided into two periods to homogenize and disperse the Ganoderma lucidum blend to obtain a primary intermediate product;
[0236] The step S35 includes:
[0237] Step S351, primary shearing stage: stirring at a speed of 1800 RPM for 1 minute to form an initial dispersion system;
[0238] Step S352, primary compensation stage: detecting the particle size distribution of the Ganoderma lucidum blend in real time, and performing compensation stirring whenever the particle size distribution is greater than a first threshold;
[0239] Step S353, secondary shear stage: stirring at 1500 RPM for 1 min to stabilize the dispersion system;
[0240] Step S354, secondary compensation stage: detecting the particle size distribution of the Ganoderma lucidum blend in real time, and performing compensatory stirring whenever the particle size distribution is greater than a second threshold;
[0241] Step S41, mixing 0.8 kg of p-hydroxyacetophenone and 2 kg of 1,2-hexanediol, and stirring in a 50° C. water bath for 15 minutes until completely dissolved, to obtain an antioxidant-moisturizing combined solvent;
[0242] Step S42, adding the antioxidant-moisturizing combined solvent to the emulsification reactor, and stirring it with the primary intermediate product at 35 RPM for 3 minutes;
[0243] Step S43: 0.5 kg of dipotassium glycyrrhizate and 5 kg of hydroxypropyl tetrahydropyrantriol are sequentially added to the emulsification reactor, stirred at 35 RPM for 3 minutes, to obtain a secondary intermediate product.
[0244] Step S51, dissolving 0.5 kg of palmitoyl tripeptide-1, 0.5 kg of palmitoyl tetrapeptide-7, and 0.5 kg of palmitoyl pentapeptide-4 in a pH 6.0 buffer solution containing 0.1 mol / L arginine, and shaking in a water bath at 45° C. for 30 min for activation;
[0245] Step S52, adding the activated palmitoyl peptide skin protective agent into the emulsification reactor;
[0246] Step S53, adding 0.5 kg of isosorbide dimethyl ether, 0.5 kg of PEG / PPG-14 / 7 dimethyl ether, 0.5 kg of succinoglycan, 0.5 kg of arginine / lysine polypeptide, 0.5 kg of hybrid rose extract, 0.5 kg of gardenia fruit extract and 0.5 kg of daily fragrance to the emulsification reactor;
[0247] Step S54, adding 1 kg of black truffle extract, 1 kg of galangal extract, 1 kg of schizonepeta tenuifolia extract, and 1.3 kg of Chinese ganoderma lucidum extract to an emulsification reactor, and stirring with the secondary intermediate product at 35 RPM for 3 minutes to obtain a primary product;
[0248] Step S55, performing online spectrum detection on the primary product;
[0249] Step S56, calculating the activity retention rates of ganoderic acid A in the Chinese Ganoderma lucidum extract, melanosporone in the Tuber melanosporum extract, spilanthol in the Spinach extract, and spilantholide in the Spinach extract based on the characteristic peak areas obtained by the online spectral detection in step S55. When the activity retention rate of any of the extracts is less than a threshold value, a compensation of the corresponding extract is added.
[0250] Step S57, adding the compensated Alpinia serrata extract, the Chinese Ganoderma lucidum extract, the Spinach nelumbo nucifera extract, and the Black Tuber extract, and stirring at 35 RPM for 3 minutes;
[0251] In step S58, stirring is maintained at 35 RPM, and the temperature is lowered to 35-38°C at a rate of 2°C / min to obtain the final product.
[0252] Step S6: sterilize and filter the final product.
[0253] Example 2
[0254] The difference between this embodiment and Example 1 is that this embodiment only changes step S54 in Example 1, and adds 2 kg of black truffle extract, 1 kg of scutellaria extract, 1 kg of schizonepeta extract and 1.3 kg of Chinese ganoderma extract into the emulsification reactor, and stirs with the secondary intermediate product at 35 RPM for 3 minutes to obtain the primary product; the rest is the same as Example 1.
[0255] Example 3
[0256] The difference between this embodiment and Example 1 is that this embodiment only changes step S54 in Example 1, and adds 1 kg of black truffle extract, 2 kg of scutellaria extract, 1 kg of scutellaria extract and 1.3 kg of Chinese ganoderma lucidum extract into the emulsification reactor, and stirs with the secondary intermediate product at 35 RPM for 3 minutes to obtain the primary product; the rest is the same as Example 1.
[0257] Example 4
[0258] The difference between this embodiment and Example 1 is that this embodiment only changes step S54 in Example 1, and adds 1 kg of black truffle extract, 1 kg of scutellaria extract, 2 kg of schizonepeta extract and 1.3 kg of Chinese ganoderma extract into the emulsification reactor, and stirs with the secondary intermediate product at 35 RPM for 3 minutes to obtain the primary product; the rest is the same as Example 1.
[0259] Example 5
[0260] The difference between this embodiment and Example 1 is that this embodiment only changes step S54 in Example 1, and adds 1 kg of black truffle extract, 1 kg of scutellaria extract, 1 kg of schizonepeta extract and 2.6 kg of Chinese ganoderma extract into the emulsification reactor, and stirs with the secondary intermediate product at 35 RPM for 3 minutes to obtain the primary product; the rest is the same as Example 1.
[0261] Example 6
[0262] The difference between this embodiment and Example 1 is that this embodiment only changes step S54 in Example 1, and adds 0.5 kg of black truffle extract, 1 kg of scutellaria extract, 1 kg of schizonepeta extract and 1.3 kg of Chinese ganoderma extract into the emulsification reactor, and stirs with the secondary intermediate product at 35 RPM for 3 minutes to obtain the primary product; the rest is the same as Example 1.
[0263] Example 7
[0264] The difference between this embodiment and Example 1 is that this embodiment only changes step S54 in Example 1, and adds 1 kg of black truffle extract, 0.5 kg of scutellaria extract, 1 kg of scutellaria extract and 1.3 kg of Chinese ganoderma extract into the emulsification reactor, and stirs with the secondary intermediate product at 35 RPM for 3 minutes to obtain the primary product; the rest is the same as Example 1.
[0265] Example 8
[0266] The difference between this embodiment and Example 1 is that this embodiment only changes step S54 in Example 1, and adds 1 kg of black truffle extract, 1 kg of scutellaria extract, 0.5 kg of scutellaria extract and 1.3 kg of Chinese ganoderma lucidum extract into the emulsification reactor, and stirs with the secondary intermediate product at 35 RPM for 3 minutes to obtain the primary product; the rest is the same as Example 1.
[0267] Example 9
[0268] The difference between this embodiment and Example 1 is that this embodiment only changes step S54 in Example 1, and adds 1 kg of black truffle extract, 1 kg of scutellaria extract, 1 kg of scutellaria extract and 0.6 kg of Chinese ganoderma extract into the emulsification reactor, and stirs with the secondary intermediate product at 35 RPM for 3 minutes to obtain the primary product; the rest is the same as Example 1.
[0269] Please see the table below for specific data.
[0270] Table 1 Component formula of the essence milk prepared in Examples 1 to 9
[0271]
[0272] Experimental results of the essence lotions of Examples 1 to 9:
[0273] In order to verify the firming effect of the skin care creams of Examples 1 to 9, the following experiments were conducted:
[0274] Using a facial image acquisition device and a skin elasticity tester, three healthy men or women aged between 30 and 60 with sagging faces were recruited for each embodiment (excluding pregnant or lactating women), for a total of 27 subjects.
[0275] The experimental steps are:
[0276] Cleansing the face with a cleansing sample in the lab;
[0277] Sit quietly in a test room at 20±1°C and 50±10% RH for more than 20 minutes without drinking water or other beverages. The subject should remain relaxed, with their face exposed and avoid being touched.
[0278] After acclimatization, the subjects were imaged before sample use, and the skin elasticity R2 value was measured using a skin elasticity tester. The test was repeated three times and the results were recorded.
[0279] Distribute test samples and provide guidance to subjects according to the sample instructions to ensure that subjects can use them correctly and continuously for 28 days;
[0280] The same pre-use image of the sample was collected 7, 14, and 28 days after the sample was used, and the skin elasticity R2 value was measured with a skin elasticity tester. The test was repeated three times and recorded. After 28 days, the subjects were revisited to conduct a follow-up questionnaire survey on sample use and self-assessment of the subject's use.
[0281] This experiment adopts the principle of randomized, self-controlled before-after experiment. The test items and evaluation criteria include:
[0282] Skin elasticity R2 value: The larger the value, the better the skin elasticity.
[0283] Lower face width: The straight line connecting the left and right mandibular angle points. The smaller the value, the better the facial lifting effect.
[0284] Nasolabial angle: The angle between the line connecting the lower nose point and the mandibular angle and the point of the mouth. The larger the value, the better the face-lift effect.
[0285] Eye Angle A: The angle between the line connecting the outer corner of the eye and the root of the nose and the nose wing on the same side. The larger the value, the better the face-lifting effect.
[0286] Eye angle B: The angle formed by the straight line connecting the inner corner of the eye and the midpoint of the eyebrow and the outer corner of the eye.
[0287] The larger the value, the better the face lifting effect.
[0288] Please see Tables 2 to 6 below for specific data.
[0289] Table 2 Experimental results of the firming effect of the essence lotion prepared in Examples 1, 2, and 3
[0290]
[0291] Table 3 Experimental results of the firming effect of the essence lotion prepared in Examples 1, 4, and 5
[0292]
[0293]
[0294] Table 4 Experimental results of the firming effect of the essence lotion prepared in Examples 1, 6, and 7
[0295]
[0296] Table 5 Experimental results of the firming effect of the essence lotion prepared in Examples 1, 8, and 9
[0297]
[0298] Table 6 Experimental results of self-assessment of the firming effect of the essence lotions prepared in Examples 1 to 9
[0299]
[0300]
[0301] It can be seen from Tables 1 to 6 above that, based on Example 1, i.e., the composition consisting of the Tuber Melanosporum extract, the Alpinia scoparia extract, the Aglaonema scoparia extract, and the Ganoderma lucidum extract in a mass ratio of 1:1:1:1.3, increasing the content of one of the extracts did not significantly improve the skin firming effect of the essence lotion. In particular, in Example 5, increasing the content of the Ganoderma lucidum extract actually reduced the skin firming effect of the essence lotion. While reducing the content of one of the extracts significantly decreased the skin firming effect of the essence lotion. In particular, in Example 9, reducing the content of the Ganoderma lucidum extract greatly reduced the skin firming effect of the essence lotion. In addition, the self-assessment of the subjects showed no improvement.
[0302] In summary, among Examples 1 to 9, the essence milk product prepared in Example 1 has the best skin firming effect, that is, the mass ratio of the black truffle extract, the forked algae extract, the spilionella extract and the Chinese ganoderma extract is 1:1:1:1.3.
[0303] So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the accompanying drawings. However, it is easy for those skilled in the art to understand that the scope of protection of the present invention is obviously not limited to these specific embodiments. Without departing from the principles of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the scope of protection of the present invention. The above is only a preferred embodiment of the present invention.
[0304] The foregoing description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Those skilled in the art will readily appreciate that the present invention is susceptible to various modifications and variations. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.
Claims
1. A skin-tightening composition, characterized in that: The composition consists of black truffle extract, forked algae extract, spilanthol extract and Chinese ganoderma lucidum extract.
2. The skin-tightening composition according to claim 1, characterized in that The mass ratio of the black truffle extract, the forked algae extract, the schisandra chinensis extract and the Chinese ganoderma lucidum extract is 1:1:1:1.
3.
3. Use of the skin-tightening composition according to any one of claims 1 to 2 in the preparation of essence lotion.
4. A method for preparing an essence milk, for preparing the essence milk according to claim 3, characterized in that: include: Step S1, adding the aqueous phase base material into an emulsification reactor and performing aqueous phase homogenization treatment to obtain an aqueous phase matrix; Step S2, melting the oil phase base material to obtain an oil phase matrix, and transferring the oil phase matrix to an emulsification reactor for emulsification to obtain an emulsified matrix; Step S3, cooling in stages and sequentially adding the primary functional components to the emulsified matrix to obtain a primary intermediate product; Step S4, adding the secondary functional components to the primary intermediate product in sequence to obtain a secondary intermediate product; Step S5, adding a composite bioactive component to obtain a final product; Step S6, sterilizing and filtering the final product; Wherein, the aqueous phase base material includes deionized water and a hydrophilic moisturizer, a thickener and an emulsion stabilizer; The oil phase base material includes C14-22 alcohol, C12-20 alkyl glucoside, sorbitan stearate, polysorbate 60 and a high temperature resistant skin protectant; The first functional component includes a pH regulator and red ganoderma extract; The second functional component includes hydroxyacetophenone, 1,2-hexanediol and a skin protectant; The composite bioactive ingredients include palmitoyl peptide skin protective agent, biological skin protective agent, fragrance, spore tuber extract, fork algae extract, schizonepeta extract and Chinese ganoderma lucidum extract.
5. The method for preparing the essence milk according to claim 4, characterized in that: The step S2 comprises: Step S21, melting C14-22 alcohol and C12-20 alkyl glucoside in an oil phase reactor at a melting temperature of 65-70° C. to obtain an initial oil phase matrix, so as to prevent the glycosidic bond breakage of the C12-20 alkyl glucoside due to local overheating when the C12-20 alkyl glucoside is mixed with other oil phase substances and heated, and to inhibit the transesterification reaction between the C14-22 alcohol and polysorbate at high temperature; Step S22, adding sorbitan stearate, polysorbate 60 and a high temperature resistant skin protectant to the oil phase reaction kettle, and stirring with the initial oil phase matrix at a low speed, the stirring temperature is divided into three stages, to obtain an oil phase matrix, wherein, In the first stage, the temperature was raised to 75°C at a rate of 0.5°C / min. The temperature was slowly raised to reduce the viscosity of the oil phase matrix, allowing sorbitan stearate to be evenly dispersed. At the same time, its HLB value (hydrophile-lipophile balance) transitioned from a solid state to a molten state, forming a gradient emulsion system with polysorbate-60. The second stage is maintained at 85°C ± 1°C for 5 minutes. The high temperature is used to convert the layered structure of alkyl glucoside and C14-22 alcohol into a cubic phase to improve the encapsulation efficiency. In the third stage, the temperature is lowered to 80°C at a rate of 1°C / min. The cooling process is used to increase the viscosity of the oil phase matrix and form an interfacial film to prevent the emulsion from merging. Step S23, transferring the oil phase matrix in the oil phase reactor to the emulsification reactor for emulsification to obtain an emulsified matrix.
6. The method for preparing the essence milk according to claim 5, characterized in that: The step S23 includes: Step S231, transferring the oil phase matrix to the emulsification reaction kettle; Step S232, using a fixed amount of deionized water to high-pressure rinse the oil phase reactor, and transferring the obtained mixture of the residual oil phase matrix and the fixed amount of deionized water to the emulsification reactor; Step S233, preliminarily mixing the oil phase matrix and the water phase matrix with low-speed stirring to obtain a water-oil blend; Step S234, measuring the viscosity of the water-oil mixture to determine the initial stirring speed of high-speed stirring and the total time of emulsification stirring; Step S235, stirring the water-oil mixture at the initial stirring speed to emulsify, and adjusting the emulsification stirring speed based on the viscosity measurement result during the emulsification process to obtain an emulsified base; Among them, the mass of the quantitative deionized water is calculated based on the mass of the deionized water in the aqueous phase base material and the total mass of the oil phase base material; the initial stirring speed is calculated based on the viscosity data measured by a viscosity measuring device at the viscosity characteristic height of the water-oil blend; the viscosity characteristic height is calculated from the volume of the aqueous phase matrix and the volume of the oil phase matrix; the total time of the emulsification stirring is calculated based on the initial stirring speed.
7. The method for preparing the essence milk according to claim 6, characterized in that: In step S235, during emulsification and stirring, the viscosity of the water-oil mixture is measured at the viscosity characteristic height at regular intervals to form a viscosity measurement curve. Based on the stability change of the viscosity measurement data per a preset unit time length, it is determined whether the viscosity measurement result within the corresponding time length is valid. If the stability change of the viscosity measurement data per the preset unit time length meets a preset stability standard, the viscosity measurement result within the corresponding time length is determined to be valid.
8. The method for preparing the essence milk according to claim 6, characterized in that: The step S3 comprises: Step S31, stirring the emulsified base at a low speed while cooling it to 70-75°C at a rate of 4°C / min; Step S32, adding a pH regulator to the emulsification reaction kettle and stirring at a low speed for 2 minutes to uniformly mix the pH regulator with the emulsification base; Step S33, stirring the emulsified base at a low speed while cooling the mixture at a rate of 4°C / min to 40-45°C; Step S34, adding the Ganoderma lucidum extract to the emulsification reaction kettle and stirring at a low speed to preliminarily mix the Ganoderma lucidum extract and the emulsification base to obtain a Ganoderma lucidum blend; Step S35, stirring the Ganoderma lucidum blend, wherein the shear force of the stirring is divided into two periods to homogenize and disperse the Ganoderma lucidum blend to obtain a primary intermediate product; The step S35 includes: Step S351, primary shearing stage: stirring at a speed of 1800 RPM for 1 minute to form an initial dispersion system; Step S352, primary compensation stage: detecting the particle size distribution value of the surface of the initial dispersion system in real time, and performing compensatory stirring whenever the particle size distribution value is greater than a first threshold value, wherein the stirring time and stirring rate of the compensatory stirring are positively correlated with the difference between the particle size distribution value and the first threshold value; Step S353, secondary shear stage: stirring at 1500 RPM for 1 minute to stabilize the dispersion system; Step S354, secondary compensation stage: Real-time detection of the particle size distribution of the dispersed system after stabilization. Whenever the particle size distribution is greater than a second threshold, compensatory stirring is performed. The stirring time and stirring rate of the compensatory stirring are positively correlated with the difference between the particle size distribution and the second threshold. The first threshold is greater than the second threshold.
9. The method for preparing the essence milk according to claim 8, characterized in that: The step S4 comprises: Step S41, p-hydroxyacetophenone and 1,2-hexanediol are mixed and stirred in a 50° C. water bath for 15 minutes until completely dissolved to obtain an antioxidant-moisturizing combined solvent; Step S42, adding the antioxidant-moisturizing combined solvent to the emulsification reactor, and stirring it with the primary intermediate product at a low speed for 3 minutes; Step S43: adding the skin protectant to the emulsification reaction kettle and stirring at a low speed for 3 minutes to obtain a secondary intermediate product.
10. The method for preparing the essence milk according to claim 9, characterized in that: The step S5 comprises: Step S51, pre-activating the palmitoyl peptide skin protective agent; Step S52, adding the activated p-palmitoyl peptide raw material into an emulsification reactor; Step S53, adding the biological skin protectant and fragrance into the emulsification reactor; Step S54, adding a composition comprising a black truffle extract, a forked algae extract, a spiltia odorifera extract, and a Chinese ganoderma lucidum extract in a mass ratio of 1:1:1:1.3 to an emulsification reactor, and stirring the mixture with the secondary intermediate product at a low speed for 3 minutes to obtain a primary product; Step S55, performing liquid online spectrum detection on the surface of the primary product; Step S56, calculating the activity retention rate of each extract based on the characteristic peak areas of ganoderic acid A in the Chinese Ganoderma lucidum extract, melanosporone in the Tuber melanosporum extract, spilanthol in the Spinach extract, and spilanthol in the Spinach extract obtained by the online spectral detection in step S55, and determining the compensation amount of each extract according to the activity retention rate, wherein the reliability of the activity retention rate is determined based on the comparison result of the characteristic peak area of each extract with the corresponding retention rate threshold; Step S57, adding the corresponding extract according to the calculated compensation amount of each extract, and stirring at a low speed; Step S58, maintaining low-speed stirring, and cooling to 35-38°C at a rate of 2°C / min to obtain the final product.
Citation Information
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