A yukon validated ancient method polymer and a preparation method thereof

Abstract

The present application relates to natural plant composite fluid preparation technical field, disclose a kind of Yu Rong efficiency test ancient method polymer and its preparation method, polymer is made of purified water, white hoelen, arrowroot, white kidney bean, white atractylodes, white tribulus terrestris, wax gourd seed, white lotus, jujube meat, gastrodia elata, dark plum, donkey-hide gelatin, pear flower, kaempferia rotunda, magnolia flower, chuanxiong, mountain gardenia and white honey.Preparation, first part purified water and dark plum, white hoelen, arrowroot and white kidney bean are heated, then supplement purified water and add the rest water extraction plant raw material for extraction;Subsequently, hydration treatment is carried out by adding donkey-hide gelatin after cooling, then aromatic plant raw material and white honey are added under lower temperature, and high shear treatment is carried out, finally defoaming and precision filtration are carried out to obtain product.The present application can reduce starch polysaccharide retrogradation aggregation and donkey-hide gelatin protein flocculation at high temperature, and reduce the volatile loss of aromatic ingredients, improve the uniformity and storage stability of fluid system.

Description

Technical Field

[0001] This invention relates to the field of natural plant composite fluid preparation technology, specifically to an ancient polymer for jade appearance verification and its preparation method. Background Technology

[0002] When preparing composite fluids from natural raw materials, it is typically necessary to transfer water-soluble components, starch polysaccharides, and aromatic or fat-soluble components from the plant materials to the aqueous phase, and to disperse protein-based raw materials such as donkey-hide gelatin in the system. For fluid systems containing both polysaccharide and protein components, polysaccharide molecular chains and protein molecules can form composite structures through hydrogen bonds and other non-covalent intermolecular interactions. These structures affect the viscosity, dispersion state, and storage stability of the system. Therefore, the processing sequence, temperature conditions, and dispersion methods of different raw materials not only affect the extraction efficiency of each component but also the composite state of polysaccharides and proteins in the liquid phase and the dispersion state of aromatic components.

[0003] Current preparation methods typically involve high-temperature extraction of various plant materials, such as donkey-hide gelatin, with water. After extraction, the mixture is then filtered, concentrated, or mechanically mixed to obtain a composite fluid. This method promotes the release of water-soluble components from the plant materials and causes starchy materials to absorb water and swell, while donkey-hide gelatin softens and dissolves. In some composite systems, polysaccharides and proteins can generate intermolecular interactions during cooling, forming a continuous aqueous phase with a certain viscosity. For systems containing aromatic plant materials, subsequent stirring can further disperse some volatile or fat-soluble components into this continuous phase, thus forming a composite fluid composed of polysaccharides, proteins, and dispersed plant-derived components.

[0004] However, existing one-time high-temperature treatment methods typically do not separately control the molecular weight changes of starch polysaccharides, protein hydration conditions, and the release and dispersion processes of aromatic components. Starch polysaccharides, without adequate degradation, tend to maintain high molecular weights and undergo retrogradation and aggregation during cooling and storage, reducing the structural stability of the polysaccharide-protein complex. Similarly, donkey-hide gelatin protein is prone to aggregation or flocculation when exposed to prolonged high temperatures, hindering the formation of a uniform polysaccharide-protein complex fluid. Furthermore, volatile and fat-soluble components in aromatic plant materials such as pear blossoms, galangal, magnolia bark flowers, and chuanxiong are easily lost under high-temperature conditions. After lowering the treatment temperature, the unbroken plant tissue restricts the migration of these components into the high-viscosity continuous phase. When only conventional mechanical stirring is used, the released aromatic components still suffer from large particle sizes and insufficient dispersion, easily leading to subsequent aggregation, sedimentation, or stratification. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides an ancient polymer for jade appearance verification and its preparation method, solving the problems of aggregation, sedimentation, stratification, and decreased storage stability of existing polymer fluids.

[0006] To address the above problems, the present invention provides the following technical solution.

[0007] In a first aspect, the present invention provides a traditional polymer for jade facial efficacy verification, employing the following technical solution: A traditional polymer for purported beauty enhancement is made from raw materials comprising the following parts by weight: Purified water 55.0–85.0 parts, Poria cocos 0.27–0.41 parts, Pueraria lobata 0.14–0.22 parts, Dolichos lablab 0.11–0.17 parts, Atractylodes macrocephala 0.14–0.22 parts, Tribulus terrestris 0.14–0.22 parts, Benincasa hispida seeds 0.19–0.29 parts, Nelumbo nucifera stamens 0.12–0.20 parts, Ziziphus jujuba pulp 0.08–0.12 parts, Astragalus membranaceus... Hemp 0.04–0.08 parts, dried plum 0.018–0.022 parts, donkey-hide gelatin 0.018–0.022 parts, pear blossom 0.06–0.10 parts, galangal 0.03–0.05 parts, magnolia bark flower 0.03–0.05 parts, chuanxiong rhizome 0.04–0.08 parts, gardenia fruit 0.03–0.05 parts, and white honey 0.018–0.022 parts.

[0008] By adopting the above technical solution, Poria cocos, kudzu root, and white hyacinth bean provide a plant matrix containing starch-based polysaccharides; Atractylodes macrocephala, Tribulus terrestris, winter melon seeds, white lotus stamens, jujube pulp, Gastrodia elata, and Gardenia jasminoides provide water-soluble or water-dispersible plant components; Prunus mume provides a source of acidic components; donkey-hide gelatin provides collagen components; pear blossom, Kaempferia galanga, Magnolia officinalis flowers, and Ligusticum chuanxiong provide aromatic and volatile plant components; and white honey participates in the structural stability of the fluid system. All raw materials are combined according to the above-mentioned mass proportions to form a raw material system suitable for staged hydrolysis, water extraction, protein hydration, and low-temperature dispersion of aromatic components.

[0009] The above raw materials are processed in stages to form a composite fluid system. The starch polysaccharides in Poria cocos, kudzu root, and white hyacinth bean undergo controlled hydrolysis, resulting in a decrease in their average molecular weight and thus reducing their tendency to re-aggregate during cooling and storage. After hydration at lower temperatures, the protein molecules of donkey-hide gelatin can form a composite system with the hydrolyzed polysaccharide segments through hydrogen bonds between polar groups such as hydroxyl and amino groups, as well as other non-covalent intermolecular interactions. The aromatic components in pear blossom, galangal, magnolia bark flower, and Ligusticum chuanxiong are released at low temperatures and dispersed under high shear, resulting in smaller particle sizes dispersed in a continuous aqueous phase. This forms a fluid system composed of polysaccharides, proteins, and aromatic dispersion components, which helps reduce the degree of aggregation, sedimentation, and stratification during storage.

[0010] Preferably, the characteristic absorption peaks of the hydroxyl and amino groups of the polymer used in the jade appearance test are located at 3311–3321 cm⁻¹, and the average particle size D50 of the dispersed phase droplets in the system is 1.8–2.4 μm.

[0011] By employing the above-mentioned technical solution, the characteristic absorption peaks of hydroxyl and amino groups fall within the aforementioned range, indicating a change in the intermolecular interaction environment of hydroxyl and amino groups in the system. This is consistent with the analytical results regarding hydrogen bonding between the polysaccharide components and donkey-hide gelatin protein. Controlling the average particle size of the dispersed phase droplets in the system within the range of 1.8–2.4 μm reduces the tendency for phase separation caused by aggregation and gravity in larger droplets, thereby improving the dispersion uniformity of the system.

[0012] Preferably, the precipitation rate of the ancient polymer used in the jade appearance test is 0.6-1.1% after centrifugation at 4000 rpm for 30 min at room temperature.

[0013] By adopting the above technical solutions, the tendency of starch polysaccharides in the system to form aggregate structures between macromolecular chains is reduced after appropriate hydrolysis. Simultaneously, the intermolecular interactions between the hydrated donkey-hide gelatin and the polysaccharide segments help reduce the degree of aggregation and sedimentation of high molecular weight components in the system. The aromatic components, after high shearing, form a dispersed phase with smaller particle sizes, which also helps reduce the sedimentation of larger dispersed particles under centrifugal conditions.

[0014] Preferably, the apparent viscosity of the Yu Rong efficacy ancient method polymer measured at 25°C and a shear rate of 10 s⁻¹ on day 60 is 92.8% to 95.1% of that on day 1.

[0015] By employing the above technical solution, the polysaccharide components undergo controlled hydrolysis in the initial stage, reducing structural changes caused by starch retrogradation during storage; the donkey-hide gelatin protein hydrates and forms intermolecular interactions with the polysaccharide components at a lower temperature; and white honey is added simultaneously with the aromatic cell-wall-breaking ultrafine powder during the high-shear stage, ensuring that sugars, polysaccharides, proteins, and aromatic dispersion components are mixed and dispersed in the same stage. This treatment method can reduce viscosity changes caused by polymer aggregation, dispersed phase coalescence, and localized phase separation during storage.

[0016] Secondly, the present invention provides a method for preparing an ancient polymer for jade facial efficacy verification, employing the following technical solution: A method for preparing an ancient polymer for jade facial efficacy testing includes the following steps: S1. Take 4.8–5.2 parts by weight of purified water, add dried plum, white poria cocos, kudzu root and white hyacinth bean, and heat at 90–95°C. After the treatment, add the remaining purified water to make the total amount of purified water 55.0–85.0 parts by weight, and add atractylodes macrocephala, tribulus terrestris, winter melon seeds, white lotus stamen, jujube pulp, gastrodia elata and gardenia fruit to continue heating and extraction. After the extraction, perform solid-liquid separation to obtain the initial extract. S2. Cool the initial extract to 55-60℃, add the pulverized donkey-hide gelatin and stir to obtain a composite fluid containing polysaccharide components and donkey-hide gelatin protein components. S3. Cool the composite fluid to 35-40°C, add pear blossoms, galangal, magnolia flower, chuanxiong and white honey that have been treated with ultra-micro cell wall breaking, and perform high shear treatment at 3500-4500 rpm; S4. The fluid after high shear treatment is allowed to stand to degas and then finely filtered. The filtrate is collected to obtain the ancient polymer for jade appearance.

[0017] By adopting the above technical solution, the water extraction, hydrolysis, protein hydration, and release and dispersion of aromatic components of the raw materials are set in different stages. The processing temperature and the order of addition are controlled according to the processing characteristics of various raw materials, so that the molecular weight adjustment of starch polysaccharides, the extraction of water-soluble plant components, the hydration of donkey-hide gelatin, and the low-temperature release and dispersion of aromatic components are carried out in their respective stages. This reduces starch retrogradation, protein aggregation, and loss of volatile components that occur when various raw materials are processed simultaneously under the same high-temperature conditions.

[0018] Preferably, in step S1, 4.8 to 5.2 parts by weight of purified water are mixed with dried plum, white poria cocos, kudzu root and white hyacinth bean, and stirred at 60 to 80 rpm for 20 to 30 minutes at 90 to 95°C.

[0019] By adopting the above technical solution, the initial water volume is controlled at 4.8–5.2 parts by mass, ensuring a high concentration of the acidic components dissolved from the plum in the local aqueous phase. The treatment temperature is controlled at 90–95°C, which promotes water absorption and swelling of starch polysaccharides and their hydrolysis under acidic conditions. A stirring speed of 60–80 rpm is used to maintain contact and mass transfer between the plant material and the aqueous phase. After treatment for 20–30 minutes, the weight-average molecular weight of the starch polysaccharide matrix can be reduced to the range shown in the examples.

[0020] Preferably, in step S1, after the heating treatment of dried plum, white poria, kudzu root and white hyacinth bean is completed, the remaining purified water is added to make the total amount of purified water reach 55.0 to 85.0 parts by mass, and white atractylodes, white tribulus, winter melon seeds, white lotus stamen, jujube pulp, gastrodia and gardenia are added. Extraction is carried out at 90 to 95℃ for 90 to 120 minutes. After extraction, non-water-soluble coarse residue is removed by centrifugation solid-liquid separation with a filtration accuracy of 80 to 100 μm.

[0021] By employing the above technical solution, starch polysaccharides are first hydrolyzed under a small amount of water, followed by the addition of purified water for the main water extraction, allowing the two treatment stages to proceed separately. The addition of water reduces the concentration of acidic components in the system, which helps control the extent of further hydrolysis of starch polysaccharides. An extraction temperature of 90–95℃ and an extraction time of 90–120 min are used to promote the entry of water-soluble components from other plant materials into the aqueous phase. After water extraction, larger insoluble plant tissues are removed by centrifugation at 80–100 μm to obtain the initial extract for subsequent hydration treatment of donkey-hide gelatin.

[0022] Preferably, the weight-average molecular weight peak of the starch polysaccharide matrix in the initial extract obtained in step S1 is 42.5–48.7 kDa.

[0023] By adopting the above technical solution, the weight-average molecular weight of the starch polysaccharide matrix in the primary extract can be controlled within the above range, which can reduce the degree of re-aggregation of macromolecular starch during cooling and storage, while retaining the thickening and structure-forming effects of polysaccharide components in the aqueous phase.

[0024] Preferably, before step S3, pear blossoms, galangal, magnolia bark flowers and chuanxiong are dried at 35-40°C until the moisture content is no more than 5.0% by mass. Then, under liquid nitrogen-assisted cooling, airflow ultrafine pulverization is carried out, and the temperature inside the pulverization chamber is controlled at -10-5°C to obtain aromatic cell wall-breaking mixed ultrafine powder with a particle size D90 of 10-15μm.

[0025] By adopting the above technical solutions, drying conditions of 35–40℃ are used to reduce the moisture content of raw materials and minimize the loss of aromatic and volatile components under high-temperature drying conditions. Controlling the moisture content to below 5.0% improves the brittle fracture degree of the material during air jet milling and reduces material adhesion and agglomeration. Using liquid nitrogen for assisted cooling during milling and controlling the milling chamber temperature between -10℃ and 5℃ reduces the temperature rise caused by mechanical action during milling, thus minimizing the volatilization loss of aromatic components. Controlling the D90 to 10–15 μm increases the specific surface area of ​​plant tissues and shortens the distance that internal components migrate to the external liquid phase.

[0026] Preferably, in step S2, the donkey-hide gelatin is pre-crushed into particles with a particle size of 1-2 mm, the initial extract is cooled to 55-60°C and then the donkey-hide gelatin particles are added, and the mixture is stirred at 120-150 rpm for 40-50 min.

[0027] By employing the above technical solution, pre-crushing the donkey-hide gelatin to 1-2 mm increases its contact area with the initial extract. At 55-60℃, the gelatin particles gradually absorb water and disperse in the initial extract, while avoiding the previous extraction temperature of 90-95℃. Stirring at 120-150 rpm promotes uniform dispersion of the gelatin particles in the initial extract and increases the contact between the gelatin protein and polysaccharide components. During the 40-50 min processing time, hydrogen bonds and other non-covalent intermolecular interactions form between the gelatin protein and polysaccharide components.

[0028] Preferably, in step S3, the composite fluid is cooled to 35-40°C, aromatic cell-wall breaking mixed ultrafine powder and white honey are added, and high shear treatment is performed at 3500-4500 rpm for 15-25 minutes.

[0029] By employing the above technical solution, a treatment temperature of 35–40°C can reduce the loss of volatile components in pear blossoms, galangal, magnolia bark flowers, and chuanxiong rhizome under high-temperature conditions. The high shear rate of 3500–4500 rpm increases the contact between the broken plant particles and the continuous aqueous phase, and allows the released lipid-soluble and aromatic components to form a micron-sized dispersed phase. Treatment for 15–25 minutes completes the mass transfer and dispersion of the aromatic components, and ensures that the average particle size of the system reaches the range shown in the examples.

[0030] Preferably, in step S4, the fluid after high shear treatment is allowed to stand for degassing for 30-40 minutes, and then finely filtered using a high-pressure plate and frame filter press.

[0031] By employing the above technical solution, static degassing is used to remove air bubbles that enter the system during the high-shear process, reducing the impact of air bubbles on subsequent fine filtration and product uniformity. Subsequently, high-pressure plate and frame filtration is used to remove residual coarse particles and insufficiently dispersed plant tissue, yielding the Yu Rong Xiao Yan ancient method polymer fluid.

[0032] This invention provides an ancient polymer for jade facial efficacy testing and its preparation method. It has the following beneficial effects: This invention employs a multi-stage process: acidic treatment with a small amount of water on starchy plant materials, hydration extraction, low-temperature hydration of donkey-hide gelatin, and low-temperature ultrafine cell disruption and high-shear dispersion of aromatic plant materials. This allows for moderate hydrolysis of starchy polysaccharides in the early stages, reducing their retroaggregation during cooling and storage. Donkey-hide gelatin is added at a lower temperature to minimize protein aggregation and flocculation caused by high-temperature treatment. Pear blossoms, galangal, magnolia bark flowers, and chuanxiong rhizome are added at low temperatures after ultrafine cell disruption, combined with high-shear treatment, to promote the release and dispersion of aromatic and fat-soluble components in the fluid system, while reducing volatilization losses caused by high-temperature extraction. This improves upon the problems of sedimentation, stratification, viscosity changes, and insufficient retention of aromatic components that easily occur in traditional single-stage high-temperature extraction processes. Attached Figure Description

[0033] Figure 1 This is a schematic diagram of the preparation process steps of the present invention; Figure 2 This is a bar chart showing the data comparison of Test Example 1 of the present invention; Figure 3 This is a bar chart showing the data comparison for Test Example 2 of the present invention. Detailed Implementation

[0034] The technical solution of the present invention will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0035] The main raw materials and reagents used in the following examples and comparative examples have the following sources and specifications. Reagents not specifically mentioned are all commercially available analytical grade or higher grade products.

[0036] This invention provides a traditional polymer for purported beauty enhancement, which is made from raw materials comprising the following parts by weight: 55.0-85.0 parts water; 0.27-0.41 parts Poria cocos, 0.14-0.22 parts Pueraria lobata, 0.11-0.17 parts Dolichos lablab, 0.14-0.22 parts Atractylodes macrocephala, 0.14-0.22 parts Tribulus terrestris, 0.19-0.29 parts Benincasa hispida seeds, and 0.12-0.20 parts Nelumbo nucifera stamens. Jujube flesh 0.08~0.12 parts, Gastrodia elata 0.04~0.08 parts; dried plum 0.018~0.022 parts; donkey-hide gelatin 0.018~0.022 parts; pear blossom 0.06~0.10 parts, galangal 0.03~0.05 parts, magnolia officinalis flower 0.03~0.05 parts, chuanxiong rhizome 0.04~0.08 parts, gardenia fruit 0.03~0.05 parts; white honey 0.018~0.022 parts.

[0037] The chemical name of purified water is water, and it refers to commercially available purified water that meets pharmacopoeia standards.

[0038] Atractylodes macrocephala, Poria cocos, Tribulus terrestris, winter melon seeds, white hyacinth bean, kudzu root, white lotus stamen, jujube flesh, pear blossom, gardenia, galangal, magnolia bark flower, Ligusticum chuanxiong, Gastrodia elata, and dried plum are all commercially available dried natural plant raw materials. The species origin and physicochemical properties of the above-mentioned plant matrix raw materials strictly meet the standard requirements stipulated in the Chinese Pharmacopoeia.

[0039] Donkey-hide gelatin is a solid, gelatinous animal collagen product made by boiling and concentrating the dried skin of donkeys (a member of the equine family) and conforms to the specifications of the Chinese Pharmacopoeia.

[0040] White honey is a white to pale yellow natural honey produced by commercially available honeybees, specifically the Chinese honeybee or the Italian honeybee, and then filtered and purified. All the aforementioned natural plant and animal ingredients are known commercial products that can be conventionally identified in this field based on their biological characteristics and pharmacopoeia physicochemical indicators; no new compound synthesis is involved.

[0041] Preparation Example 1: This preparation example provides a method for preparing aromatic cell wall-breaking mixed ultrafine powder, including the following steps: Weigh out 0.08 parts of pear blossom, 0.04 parts of galangal, 0.04 parts of magnolia flower, and 0.06 parts of chuanxiong rhizome according to the specified mass ratio. Place the above materials in a vacuum drying oven and dry them at a constant temperature of 37℃ until the moisture content of the materials is ≤5.0%. Put the dried materials into a pre-cooled supersonic airflow pulverizer for ultra-fine physical cell wall breaking pulverization. During the pulverization process, liquid nitrogen refrigerant is introduced to assist in cooling, and the temperature inside the pulverization chamber is controlled to be constant at 0℃. Adjust the speed of the airflow pulverizer classifier to 3000 rpm, and collect the aromatic cell wall breaking mixed ultra-fine powder with a particle size D90 of 12μm through a cyclone separation system. Store it in a sealed container away from light for later use.

[0042] Preparation Example 2: This preparation example provides a method for preparing aromatic cell wall-breaking mixed ultrafine powder, including the following steps: Weigh out 0.08 parts of pear blossom, 0.04 parts of galangal, 0.04 parts of magnolia bark flower, and 0.06 parts of chuanxiong rhizome according to the specified mass ratio. Place the above materials in a vacuum drying oven and dry them at a constant temperature of 35℃ until the moisture content of the materials is ≤5.0%. Put the dried materials into a pre-cooled supersonic airflow pulverizer for ultra-fine physical cell wall breaking pulverization. During the pulverization process, liquid nitrogen refrigerant is introduced to assist in cooling, and the temperature inside the pulverization chamber is controlled to be constant at -10℃. Adjust the speed of the airflow pulverizer classifier to 3500 rpm, and collect the aromatic cell wall breaking mixed ultra-fine powder with a particle size D90 of 10μm through a cyclone separation system. Store it in a sealed container away from light for later use.

[0043] Preparation Example 3: This preparation example provides a method for preparing aromatic cell wall-breaking mixed ultrafine powder, including the following steps: Weigh out 0.08 parts of pear blossom, 0.04 parts of galangal, 0.04 parts of magnolia bark flower, and 0.06 parts of chuanxiong rhizome according to the specified mass ratio. Place the above materials in a vacuum drying oven and dry them at a constant temperature of 40℃ until the moisture content of the materials is ≤5.0%. Put the dried materials into a pre-cooled supersonic airflow mill for ultrafine physical cell wall breaking and pulverization. During the pulverization process, liquid nitrogen refrigerant is introduced to assist in cooling, and the temperature inside the pulverization chamber is controlled to be constant at 5℃. Adjust the speed of the airflow milling classifier to 2500 rpm, and collect the aromatic cell wall breaking mixed ultrafine powder with a particle size D90 of 15μm through a cyclone separation system. Store it in a sealed container away from light for later use. Example

[0044] This embodiment provides a method for preparing a traditional polymer for jade facial efficacy testing, employing optimized core process parameters, as detailed in the appendix. Figure 1 This includes the following steps: Weigh the following ingredients according to the specified proportions: 69.14 parts purified water, 0.18 parts Atractylodes macrocephala, 0.34 parts Poria cocos, 0.18 parts Tribulus terrestris, 0.24 parts Benincasa hispida seeds, 0.14 parts Dolichos lablab, 0.18 parts Pueraria lobata, 0.16 parts Nelumbo nucifera stamens, 0.10 parts Ziziphus jujuba pulp, 0.08 parts Pyrus pyrifolia flowers, 0.04 parts Gardenia jasminoides, 0.04 parts Kaempferia galanga, 0.04 parts Magnolia officinalis flowers, 0.06 parts Ligusticum chuanxiong, 0.06 parts Gastrodia elata, 0.02 parts Colla corii asini, 0.02 parts Prunus mume, and 0.02 parts honey.

[0045] Material pretreatment: Prepare aromatic cell-wall broken mixed ultrafine powder (containing the prescribed amounts of pear blossom, galangal, magnolia bark flower, and chuanxiong) according to the method of Preparation Example 1 for later use. Mechanically pulverize the prescribed amount of donkey-hide gelatin into particles with a particle size of 1-2 mm at room temperature for later use.

[0046] Phase 1: Add 5.0 parts of purified water to a composite reactor equipped with a jacketed temperature control and a bottom high-shear homogenizing emulsifier. Then add the prescribed amounts of dried plum, white poria cocos, kudzu root, and white hyacinth bean. Turn on the jacket heating to raise the temperature of the system inside the reactor to 95°C. Maintain the temperature under a sealed environment and stir at 70 rpm for 25 minutes to allow the system to complete the micro-hydrolysis of amylose in a locally high-concentration acidic microenvironment. Subsequently, add the remaining 64.14 parts of purified water to the reactor and add the prescribed amounts of atractylodes macrocephala, tribulus terrestris, winter melon seeds, white lotus stamens, jujube pulp, gastrodia elata, and gardenia fruit. Maintain the system temperature at 95°C and reflux for 105 minutes. After extraction, separate the solid and liquid components of the mixture in the reactor using a centrifuge with a filtration precision of 100 μm to remove non-water-soluble crude residue. Return the initial extract to the reactor.

[0047] Phase Two: Turn on the cooling water in the reactor jacket to cool the fluid system inside the reactor and stabilize it at 58°C. Slowly add the pretreated donkey-hide gelatin granules into the reactor, adjust the speed of the anchor-type stirrer to 135 rpm, and maintain this temperature parameter for 45 minutes to allow the collagen water to merge with the polysaccharide dextrin network and complete hydrogen bond grafting.

[0048] Phase 3: Continue cooling to reduce the fluid temperature inside the reactor to 38°C and maintain it constant. Add the aromatic cell-wall-breaking mixed ultrafine powder and the prescribed amount of white honey. Turn off the low-speed stirring and turn on the high-shear homogenizing emulsifier head at the bottom of the reactor, adjusting the speed to 4000 rpm for 20 minutes of high-intensity mechanical shearing and mass transfer emulsification. After completion, stop stirring and allow the system to stand at 38°C for 35 minutes to degas. Finally, use a high-pressure plate and frame filter press (filter material pore size 3μm) to finely filter the fluid, and collect the filtrate to obtain the target polymer fluid. Example

[0049] This embodiment provides a method for preparing a traditional polymer for jade facial efficacy verification, using a combination of lower limit process parameters, including the following steps: Weigh the following ingredients according to the specified proportions: 55.0 parts purified water, 0.14 parts Atractylodes macrocephala, 0.27 parts Poria cocos, 0.14 parts Tribulus terrestris, 0.19 parts Benincasa hispida seeds, 0.11 parts Dolichos lablab, 0.14 parts Pueraria lobata, 0.12 parts Nelumbo nucifera stamens, 0.08 parts Ziziphus jujuba pulp, 0.06 parts Pyrus pyrifolia flowers, 0.03 parts Gardenia jasminoides, 0.03 parts Kaempferia galanga, 0.03 parts Magnolia officinalis flowers, 0.04 parts Ligusticum chuanxiong, 0.04 parts Gastrodia elata, 0.018 parts Colla corii asini, 0.018 parts Prunus mume, and 0.018 parts honey.

[0050] Material pretreatment: Prepare aromatic cell-wall broken mixed ultrafine powder according to the method of Preparation Example 2. Crush the prescribed amount of donkey-hide gelatin into particles with a particle size of about 1 mm for later use.

[0051] Phase 1: Add 4.8 parts of purified water to the composite reactor, along with the prescribed amounts of dried plum, poria cocos, kudzu root, and white hyacinth bean. Heat to 90℃, seal and maintain the temperature at 60 rpm for 30 minutes. Then, add the remaining 50.2 parts of purified water to the reactor, along with the prescribed amounts of atractylodes macrocephala, tribulus terrestris, winter melon seeds, white lotus stamens, jujube pulp, gastrodia elata, and gardenia fruit. Maintain the system temperature at 90℃ and reflux for 120 minutes. Separate the mixture in the reactor using a centrifuge with an 80μm filtration precision, and return the initial extract to the reactor.

[0052] Phase Two: Cool the fluid system inside the vessel and stabilize it at 55℃. Add the donkey-hide gelatin granules to the vessel, adjust the stirring speed to 120 rpm, and maintain this temperature parameter for 50 minutes.

[0053] Phase 3: Reduce the temperature of the fluid inside the reactor to 35°C and maintain it constant. Add the aromatic cell-wall breaking and mixing ultrafine powder and white honey. Turn on the high-shear homogenizing emulsifier head, adjust the speed to 3500 rpm, and perform mechanical shearing for 25 minutes. Let it stand for degassing for 40 minutes, then use a high-pressure plate and frame filter press to finely filter the fluid. Collect the filtrate to obtain the target polymer fluid. Example

[0054] This embodiment provides a method for preparing a traditional polymer for jade facial efficacy verification, using an upper limit combination of process parameters, including the following steps: Weigh the following ingredients according to the specified proportions: 85.0 parts purified water, 0.22 parts Atractylodes macrocephala, 0.41 parts Poria cocos, 0.22 parts Tribulus terrestris, 0.29 parts Benincasa hispida seeds, 0.17 parts Dolichos lablab, 0.22 parts Pueraria lobata, 0.20 parts Nelumbo nucifera stamens, 0.12 parts Ziziphus jujuba pulp, 0.10 parts Pyrus pyrifolia flowers, 0.05 parts Gardenia jasminoides, 0.05 parts Kaempferia galanga, 0.05 parts Magnolia officinalis flowers, 0.08 parts Ligusticum chuanxiong, 0.08 parts Gastrodia elata, 0.022 parts Colla corii asini, 0.022 parts Prunus mume, and 0.022 parts honey.

[0055] Material pretreatment: Prepare aromatic cell-wall broken mixed ultrafine powder according to the method of Preparation Example 3. Crush the prescribed amount of donkey-hide gelatin into particles with a particle size of about 2 mm for later use.

[0056] Phase 1: Add 5.2 parts of purified water to the composite reactor, along with the prescribed amounts of dried plum, white poria cocos, kudzu root, and white hyacinth bean. Heat to 95℃, seal and maintain the temperature at 80 rpm for 20 minutes. Then, add the remaining 79.8 parts of purified water to the reactor, along with the prescribed amounts of atractylodes macrocephala, tribulus terrestris, winter melon seeds, white lotus stamens, jujube pulp, gastrodia elata, and gardenia fruit. Maintain the system temperature at 95℃ and reflux for 90 minutes. Separate the solid and liquid components of the mixture in the reactor using a centrifuge with a filtration precision of 100 μm, and return the initial extract to the reactor.

[0057] Phase Two: Cool the fluid system inside the vessel and stabilize it at 60℃. Add the donkey-hide gelatin granules to the vessel, adjust the stirring speed to 150 rpm, and maintain this temperature parameter for 40 minutes.

[0058] Phase 3: Reduce the temperature of the fluid inside the reactor to 40℃ and maintain it constant. Add aromatic cell-wall breaking and ultrafine powder and white honey. Turn on the high-shear homogenizing emulsifier head, adjust the speed to 4500 rpm, and perform mechanical shearing for 15 minutes. Let it stand for degassing for 30 minutes, then use a high-pressure plate and frame filter press to finely filter the fluid. Collect the filtrate to obtain the target polymer fluid.

[0059] Comparative Example 1: Compared with Example 1, the difference lies in the use of a traditional one-time heating extraction process for all components. Specifically, 69.14 parts of purified water and all materials (including pretreated aromatic cell-wall-breaking mixed ultrafine powder and donkey-hide gelatin) are added to the reaction vessel at one time, and extracted under constant temperature reflux at 95°C for 105 minutes. After cooling and filtration, the product is obtained. The rest of the formula is the same.

[0060] Comparative Example 2: Compared to Example 1, the difference lies in that the purified water was not physically separated in Stage 1. Specifically, in Stage 1, all 69.14 portions of purified water were directly mixed and heated with the prescribed amounts of dried plum, white poria, kudzu root, and white hyacinth bean, without any subsequent addition of purified water. The timing and parameters of the remaining additions were the same.

[0061] Comparative Example 3: Compared with Example 1, the difference is that the aromatic guest materials (pear blossom, galangal, magnolia bark flower, and chuanxiong) added in Stage 3 were not subjected to ultra-micro cell wall breaking pretreatment, but were directly used as conventional slices or coarse powder (about 40 mesh). The other addition sequence and parameters are the same.

[0062] Comparative Example 4: Compared to Example 1, the difference lies in that the high-shear homogenizing emulsifier was not activated in Stage 3. Specifically, after cooling to 38°C and feeding the materials, only an anchor-type agitator was used for low-speed mechanical stirring at 100 rpm for 20 minutes, while the rest of the feeding sequence and parameters remained the same.

[0063] Comparative Example 5: Compared to Example 1, the difference lies in the timing of the addition of the rheological end modifier (white honey). Specifically, white honey is not added during the high-shear cooling mass transfer process in Stage 3. Instead, after the final fluid is finely filtered and discharged, 0.02 parts of white honey are added to the filtrate at room temperature and simply mechanically stirred to mix. All other parameters remain the same.

[0064] Test Example 1: (1) The initial extracts after the completion of stage one of each embodiment and the intermediate fluids of the corresponding stages of each comparative example were filtered through a 0.45 μm microporous membrane. The weight-average molecular weight distribution peak of the starch polysaccharide matrix was determined using a gel permeation chromatography (GPC) system equipped with a differential refractive index detector at a flow rate of 0.6 mL / min and a column temperature of 35 °C.

[0065] (2) The polymer fluid samples prepared in each group were freeze-dried, ground, and then prepared by KBr pelleting. The samples were scanned in the wavenumber range of 4000 cm⁻¹ to 400 cm⁻¹ with a resolution of 4 cm⁻¹. The scans were accumulated 32 times. The peak position changes of the characteristic absorption peaks in the hydroxyl and free amino regions were recorded using Fourier transform infrared spectroscopy (FTIR) to investigate hydrogen bond interactions.

[0066] (3) Referring to GB / T38104-2019 and related general industry evaluation methods for the physical stability of colloidal fluids, take 50 mL of the final polymer fluid sample and place it in a standard centrifuge tube. Centrifuge at 4000 rpm for 30 min at room temperature using a benchtop high-speed centrifuge. Carefully aspirate the supernatant, collect the bottom precipitate and dry it in an oven until constant weight. Weigh and calculate the percentage of the precipitate mass to the total mass of the original fluid sample.

[0067] (4) Take the final products of each group and place them in a constant temperature sample retention room (25℃±1℃) to stand in the dark. On the 1st and 60th day after sample preparation, the apparent viscosity of the system is measured by rotational rheometer at 25℃ and constant shear rate of 10s-1. The retention rate of viscosity on the 60th day relative to the initial viscosity on the 1st day is calculated.

[0068] Example 1 45.2 3315 0.8 94.3 Example 2 48.7 3321 1.1 92.8 Example 3 42.5 3311 0.6 95.1 Comparative Example 1 185.6 3389 14.5 45.2 Comparative Example 2 178.4 3342 12.8 61.4 Comparative Example 5 44.8 3365 4.7 58.7 From Table 1 and Figure 2 The test results show that the molecular weight of the polysaccharides in the initial extracts of Examples 1 to 3 (42.5 kDa to 48.7 kDa) is significantly lower than that of Comparative Examples 1 and 2 (approximately 178 kDa to 185 kDa). This indicates that the initial boiling of the plums with a small amount of water is effective. This operation locally increases the acidity of the system, causing the long chains of amylose to be broken down and undergoing moderate hydrolysis and degradation. In Comparative Example 2, because all the water was added at once, the acidity of the plums was diluted and buffered by the large amount of water and other materials, failing to reach the pH value required for hydrolysis. The starch was not effectively degraded, remaining in a large molecular state, and easily recrystallized and aged after cooling, resulting in a centrifugal sedimentation rate of up to 12.8% in the final product.

[0069] Based on the Fourier Transform Infrared (FTIR) data, the absorption peaks of the hydroxyl and amino groups in the Example Group were between 3311 cm⁻¹ and 3321 cm⁻¹, showing a significant red shift compared to Comparative Example 1. This indicates that after adding the donkey-hide gelatin at a temperature of around 50 degrees Celsius, the amino groups of the donkey-hide gelatin protein did indeed bind with the dextrin hydroxyl groups produced by the previous hydrolysis, forming a relatively stable hydrogen bond network. In contrast, although the starch in Comparative Example 5 was also hydrolyzed normally in the early stages, its absorption peak remained at 3365 cm⁻¹. This shows that if the white honey is simply stirred in at room temperature at the end, it cannot truly integrate into this polymer network. Due to the lack of forced mixing with a high-shear device, the white honey cannot provide end-capping protection, and the system structure becomes loose over time. Therefore, after 60 days, the viscosity of Comparative Example 5 dropped significantly, with a retention rate of only 58.7%.

[0070] From the perspective of conventional physicochemical indicators, the centrifugal sedimentation rate of the samples prepared in the examples was controlled within 1.1%, and the viscosity retention rate after 60 days was above 92.8%, which fully meets the requirements of relevant industry standards for the state and stability of such products. These data collectively confirm the feasibility of the process design of this invention: first, water is added in steps for localized acid hydrolysis; then, the temperature is lowered and donkey-hide gelatin is added to prevent high-temperature denaturation of the protein; finally, high-shear addition of white honey completes the structural end-capping. By adjusting the order of addition and temperature, the engineering problems of starch aging and crystallization and protein thermal flocculation are effectively avoided, and the resulting product maintains excellent homogeneity and stability even after long-term storage.

[0071] Test Example 2: (1) Accurately measure 5.0 mL of the final polymer fluid sample prepared in each example and comparative example, place it in a 50 mL stoppered centrifuge tube, and add 25 mL of methanol. Use a CNC ultrasonic cleaner (250 W power, 40 kHz frequency) to ultrasonically treat the sample for 45 min at room temperature to disrupt the colloidal network of the polymer fluid and fully extract the lipid-soluble volatile components. After extraction, centrifuge the tube at 5000 rpm for 15 min, collect the supernatant, filter it through a 0.22 μm microporous membrane, and use the filtrate as the test solution.

[0072] (2) Referring to the General Rules of Part IV of the 2020 Edition of the Chinese Pharmacopoeia and the industry's routine chromatographic analysis standards, the absolute content of tetramethylpyrazine in the test solution was determined by high performance liquid chromatography (HPLC). The chromatographic conditions were set as follows: octadecylsilane-bonded silica column (C18, 250 mm × 4.6 mm, 5 μm); methanol-water (45:55 v / v) as the mobile phase; flow rate of 1.0 mL / min; detection wavelength of 277 nm; column temperature of 30 °C; and injection volume of 10 μL. The mass concentration of tetramethylpyrazine was calculated by the external standard method.

[0073] (3) Take an appropriate amount of the final product fluid from each group, and extract the total volatile oil using Soxhlet extraction combined with steam distillation. After dehydration with anhydrous sodium sulfate, accurately weigh the oil and calculate the total retention rate of volatile oil (based on the percentage conversion of theoretical feed amount).

[0074] (4) Take the final product fluids from each group and use a laser particle size analyzer to determine the average particle size (D50) of the dispersed phase droplets in the system. Before the measurement, the fluid samples are appropriately diluted with purified water, and the shading is controlled within the range of 8% to 12%. The refractive index parameter is set according to the plant emulsion model inside the instrument. The particle size data is recorded to characterize the dispersion state of the microemulsion system.

[0075] Example 1 15.6 88.4 2.1 Example 2 14.9 86.2 2.4 Example 3 16.1 89.1 1.8 Comparative Example 1 3.2 18.5 45.2 Comparative Example 3 1.5 8.4 32.6 Comparative Example 4 5.4 26.7 18.5 Combined with Table 2 and Figure 3 The test data showed that the concentration of tetramethylpyrazine in Examples 1 to 3 ranged from 14.9 mg / L to 16.1 mg / L, with a total volatile oil retention rate of over 86%. In contrast, in Comparative Example 1, which used conventional one-pot heating, the concentration of tetramethylpyrazine was only 3.2 mg / L, with a retention rate of less than 20%. This indicates that traditional high-temperature extraction causes a large amount of heat-sensitive, fat-soluble components to escape with the water vapor. By adding the volatile aromatic materials at the end after cooling to 35°C to 40°C, avoiding the high-temperature environment, we effectively reduced volatilization losses.

[0076] Furthermore, the data for Comparative Example 3 was extremely low, with a ligustrazine concentration of only 1.5 mg / L. This is because the viscosity of the entire system was already very high after cooling. Without physical disruption of the tightly structured medicinal materials like ligustrazine and kaempferia galanga, the intact cell walls would block the active ingredients, preventing the volatile oils from being extracted and diffused into the viscous aqueous phase. The example used airflow ultrafine grinding to break down the cell walls, directly exposing the active ingredients and transforming the previously difficult internal diffusion into direct surface dissolution, thus solving the problem of extracting active ingredients under low-temperature, high-viscosity conditions.

[0077] Looking at the role of the high-shear equipment, although Comparative Example 4 also added cell-wall breaking powder, it only used low-speed stirring, and the concentration of tetramethylpyrazine was only 5.4 mg / L, with an average particle size of 18.5 μm. This indicates that under low-temperature and high-viscosity conditions, ordinary stirring is insufficient to break down the volatile oil, which cannot be evenly dispersed after extraction and cannot be stabilized in the aqueous phase. The example used a high-shear emulsification head operating at over 3500 rpm, using powerful mechanical shear force to directly break down the volatile oil into droplets of approximately 2 μm. In this mixing process, the polysaccharide and protein network prepared in the first two steps acted as emulsifiers, encapsulating these small droplets and forming a stable emulsion. The final test results also met relevant industry standards, confirming that the operation of ultra-micro cell-wall breaking combined with high-shear emulsification effectively solved the practical production problems of volatile oil not being extracted or retained in traditional processes.

[0078] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A polymer for verifying the efficacy of jade-like skin, characterized in that, Made from the following ingredients in parts by weight: Water 55.0–85.0 parts, Poria cocos 0.27–0.41 parts, Pueraria lobata 0.14–0.22 parts, Dolichos lablab 0.11–0.17 parts, Atractylodes macrocephala 0.14–0.22 parts, Tribulus terrestris 0.14–0.22 parts, Benincasa hispida seeds 0.19–0.29 parts, Nelumbo nucifera stamens 0.12–0.20 parts, Ziziphus jujuba pulp 0.08–0.12 parts, Gastrodia elata 0.04–0.08 parts, dried plum 0.018–0.022 parts, donkey-hide gelatin 0.018–0.022 parts, pear blossom 0.06–0.10 parts, galangal 0.03–0.05 parts, magnolia bark flower 0.03–0.05 parts, chuanxiong rhizome 0.04–0.08 parts, gardenia fruit 0.03–0.05 parts, and white honey 0.018–0.022 parts.

2. The ancient polymer for verifying facial beauty according to claim 1, characterized in that: The polymer has hydroxyl / amino characteristic absorption peaks at 3311–3321 cm⁻¹, a centrifugal sedimentation rate of 0.6–1.1%, and a retention rate of 92.8–95.1% of the apparent viscosity on day 60 relative to that on day 1. The average particle size D50 of the dispersed phase droplets in the system is 1.8–2.4 μm. The centrifugal sedimentation rate was measured at 4000 rpm for 30 min at room temperature; the apparent viscosity was measured at 25°C and a shear rate of 10 s⁻¹.

3. A method for preparing an ancient polymer for jade facial verification, used to prepare the ancient polymer for jade facial verification as described in any one of claims 1-2, characterized in that, Includes the following steps: S1. Mix part of the purified water with dried plum, white poria, kudzu root and white hyacinth bean and heat it. Then add the remaining purified water to the total amount required by the formula, and add atractylodes macrocephala, tribulus terrestris, winter melon seeds, white lotus stamen, jujube pulp, gastrodia elata and gardenia fruit for heating and extraction. After extraction, perform solid-liquid separation to obtain the initial extract. S2. Cool the initial extract, add crushed donkey-hide gelatin and stir to obtain a composite fluid; S3. Further cool the composite fluid, add pear blossoms, galangal, magnolia flower, chuanxiong and white honey that have been treated with ultra-micro cell wall breaking, and perform high shear treatment to obtain emulsified fluid; S4. The emulsified fluid is allowed to stand to defoam and then finely filtered. The filtrate is collected to obtain the ancient polymer for jade appearance efficacy.

4. The preparation method of the ancient polymer for jade facial efficacy according to claim 3, characterized in that: Before step S3, pear blossoms, galangal, magnolia bark flowers, and chuanxiong undergo ultrafine cell wall disruption pretreatment, which includes: Pear blossoms, galangal, magnolia bark flowers, and chuanxiong were dried at 35–40℃ until the moisture content was ≤5.0%. Then, they were subjected to airflow ultrafine grinding under liquid nitrogen-assisted cooling conditions, with the temperature inside the grinding chamber controlled at -10–5℃, to obtain aromatic cell wall-breaking mixed ultrafine powder with a particle size D90 of 10–15 μm.

5. The method for preparing an ancient polymer for jade facial efficacy according to claim 3, characterized in that: In step S1, 4.8 to 5.2 parts by weight of purified water are mixed with dried plum, white poria cocos, kudzu root and white hyacinth bean, and stirred at 60 to 80 rpm for 20 to 30 minutes at 90 to 95°C.

6. The method for preparing an ancient polymer for jade facial verification according to claim 3, characterized in that: In step S1, after the heating treatment of dried plum, white poria, kudzu root and white hyacinth bean is completed, the remaining purified water is added to the total amount required by the formula, and white atractylodes, white tribulus, winter melon seeds, white lotus stamen, jujube pulp, gastrodia and gardenia are added. The mixture is heated and extracted at 90-95℃ for 90-120 minutes. After extraction, non-water-soluble coarse residue is removed by centrifugation solid-liquid separation with a filtration accuracy of 80-100μm.

7. The method for preparing an ancient polymer for jade facial verification according to claim 3, characterized in that: The weight-average molecular weight peak of the starch polysaccharide matrix in the initial extract obtained in step S1 is 42.5–48.7 kDa.

8. The method for preparing an ancient polymer for jade facial verification according to claim 3, characterized in that: In step S2, the donkey-hide gelatin is pre-crushed into particles with a particle size of 1-2 mm. The initial extract is cooled to 55-60°C and then the donkey-hide gelatin particles are added. The mixture is stirred at a speed of 120-150 rpm for 40-50 minutes.

9. The preparation method of the ancient polymer for jade facial efficacy according to claim 3, characterized in that: In step S3, the composite fluid is cooled to 35-40°C, aromatic cell wall breaking mixed ultrafine powder and white honey are added, and high shear treatment is performed at a speed of 3500-4500 rpm for 15-25 minutes.

10. The method for preparing an ancient polymer for jade facial verification according to claim 3, characterized in that: In step S4, the emulsified fluid is allowed to stand at 35-40°C for 30-40 minutes to defoam and then subjected to fine filtration; wherein the fine filtration adopts a high-pressure plate and frame filter press.

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