A dietary therapy formula and preparation method for a kidney-tonifying and hair-darkening beverage
By constructing a composite colloidal buffer aqueous phase and using high-shear emulsification technology, the problems of flocculation and phase separation when mixing black bean extract and mulberry extract were solved, achieving long-term stability and homogeneity of the beverage and avoiding sedimentation and stratification.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- JIALE (SHANDONG) HOLDINGS CO LTD
- Filing Date
- 2026-04-14
- Publication Date
- 2026-07-10
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Figure CN122350239A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of food processing technology, specifically to a dietary therapy formula for a kidney-tonifying and hair-darkening beverage and its preparation method. Background Technology
[0002] Black beans, polygonatum, mulberries, and black sesame seeds, as traditional food and medicinal ingredients, are often combined in the development of nutritional supplements. However, in actual industrial production, blending these raw materials with different physicochemical properties into a liquid system presents complex challenges in terms of physicochemical stability. Black bean extract is rich in phytoglobulins, while mulberry extract is rich in various organic acids, exhibiting strong acidity. When these two materials are directly mixed, the proton concentration within the system changes drastically. Once the ambient pH decreases and approaches the isoelectric point of black bean protein, the net charge on the surface of the protein molecules rapidly approaches zero, leading to a significant weakening of the electrostatic repulsion between molecules. The free protein molecules then irreversibly aggregate and flocculate due to van der Waals forces.
[0003] This protein phase transition triggered by acidic components not only disrupts the homogeneity of the aqueous system but also triggers a chain reaction of emulsification instability. The cold-pressed black sesame oil introduced into the formula, as a hydrophobic phase, is highly susceptible to collisions between oil droplets after the proteins aggregate and lose their original interfacial activity support. Conventional food and beverage processing typically relies on adding a single thickener to increase liquid viscosity or only performing basic mechanical stirring and homogenization. These conventional techniques cannot prevent the direct impact of free protons on protein amino acid residues at the microscopic level, nor can they construct a sufficiently strong steric barrier at the complex oil-water-solid multiphase interface. After reaching shelf life, the resulting product is prone to bottom precipitation, upper fat accumulation, and overall stratification due to gravity and thermodynamic instability, failing to maintain a long-term homogeneous state and severely restricting the industrial application and quality control of such compound plant-based beverages. Summary of the Invention
[0004] To address the shortcomings of existing technologies, this invention provides a dietary formula for a kidney-tonifying and hair-darkening beverage and its preparation method, solving the problems of isoelectric point flocculation and phase separation that exist when plant proteins are compounded with acidic fruit juices. When plant proteins approach their isoelectric point, the net surface charge tends to zero, and the electrostatic repulsion weakens. At this point, irreversible aggregation and precipitation between molecules are very likely to occur.
[0005] To address the above problems, the present invention provides the following technical solution:
[0006] In a first aspect, the present invention provides a dietary therapy formula for a kidney-tonifying and hair-darkening beverage, employing the following technical solution:
[0007] A dietary therapy recipe for a kidney-tonifying and hair-darkening drink, made from the following ingredients in parts by weight:
[0008] The mixture comprises: 150-250 parts black soybean protein extract; 80-120 parts Polygonatum sibiricum polysaccharide extract; 40-60 parts mulberry concentrated juice; 20-40 parts cold-pressed black sesame oil; 1.5-2.5 parts sodium stearoyl lactylate; 1.0-2.0 parts sodium alginate; 0.3-0.8 parts sodium hexametaphosphate; 0.8-1.2 parts potassium citrate monohydrate; 0.2-0.4 parts dipotassium glycyrrhizate; and 560-730 parts softened water. The sodium alginate, sodium hexametaphosphate, and potassium citrate monohydrate form a network hydration layer in the aqueous phase, which spatially encapsulates the free protein in the black soybean protein extract and the droplets of cold-pressed black sesame oil.
[0009] By adopting the above technical solution, a composite colloidal buffer aqueous phase is constructed by using a specific ratio of sodium alginate, sodium hexametaphosphate, and potassium citrate monohydrate, combined with sodium stearoyl lactylate which has surface activity. Therefore, the effect of resisting protein flocculation induced by acidic components and maintaining the long-term stability of the emulsion is obtained.
[0010] This stabilizing effect relies on multi-dimensional physicochemical synergy within the system, and its microscopic reaction mechanism proceeds according to the following process:
[0011] Step 1, Buffer System Construction and Ion Masking: Potassium citrate monohydrate dissociates in the aqueous phase to generate citrate ions, establishing a Cit... 3- +H + ⇌HCit 2- It maintains the weak acid salt buffer balance. At the same time, sodium hexametaphosphate releases polyphosphate ions, which complex with free calcium, magnesium and other polyvalent metal cations, eliminating the salting-out cross-linking effect of polyvalent metal ions on protein and polysaccharide molecules.
[0012] Step 2, Construction of the hydration layer: Sodium alginate molecules are fully hydrated and extended under heating and stirring. The uronic acid groups on its main chain are negatively charged and form a uniform linear polyanionic polymer network under the dispersion effect of sodium hexametaphosphate.
[0013] Step 3, Multiphase Encapsulation and Proton Absorption: After black soybean protein extract and black sesame cold-pressed oil are mixed into the system, sodium stearoyl lactylate is oriented at the oil-water interface to reduce interfacial tension, and the sodium alginate polymer network encapsulates the protein molecules and oil droplets within the network. When acidic mulberry concentrate is introduced, the released protons first bind to citrate ions in the aqueous phase, slowing down the rate of decrease in the global pH value. Simultaneously, the steric barrier formed by sodium alginate around the free protein blocks direct collisions between protons and amino acid residues on the protein molecule surface, preventing the protein molecule charge from dropping to the isoelectric point range, thereby avoiding protein molecule aggregation due to van der Waals forces.
[0014] Preferably, the system obtained from the dietary therapy formula is an oil-in-water emulsion, and the droplets formed by the dispersion of the cold-pressed black sesame oil in the oil-in-water emulsion have an average particle size of 0.3 μm to 1 μm.
[0015] By adopting the above technical solution, since the average particle size of the oil phase droplets is controlled at the submicron level, according to Stokes' law, the Brownian motion force on the droplets is sufficient to resist the sedimentation and floating tendency caused by gravity. Therefore, the effect of enhancing the dynamic stability of the dispersed phase in the continuous phase is obtained, effectively avoiding the phenomenon of water separation and fat floating in the finished product during the shelf life.
[0016] Preferably, the mass centrifugation sedimentation rate of the finished product obtained from the dietary therapy formula is 0.5% to 1.6%, and the pH difference of the dietary therapy formula before and after mixing with the mulberry concentrate is 0.05 to 0.15.
[0017] By adopting the above technical solution, the buffer mesh inside the system absorbs free hydrogen ions and transforms the large fluctuations in the pH of the system into a smooth transition. Therefore, it achieves the effect of controlling the pH difference and significantly reducing the centrifugal sedimentation rate, which macroscopically confirms the anti-flocculation ability under the synergistic effect of microscopic spatial steric hindrance and ion buffering.
[0018] Preferably, the black soybean protein extract is prepared by the following steps: Non-GMO black soybeans are pulverized through a 60-mesh sieve to obtain black soybean powder. The black soybean powder is mixed with softened water at a mass-to-volume ratio of 1:8-1:12 g / mL and slurry is prepared. A 5% sodium bicarbonate aqueous solution is added dropwise to adjust the pH of the system to 8-8.4. The extract is mechanically stirred and extracted for 1.5-2.5 hours in a constant temperature water bath at 40-50℃. After extraction, the extract is centrifuged at 5000 r / min for 15 minutes, and the supernatant is collected. A 5% anhydrous citric acid aqueous solution is added dropwise to adjust the pH of the supernatant back to 7. The supernatant is concentrated by vacuum rotary evaporation or by adding softened water to adjust the soluble solids mass fraction to 8%-10%. The extract is then sterilized in an autoclave at 121℃ for 15 minutes to obtain the final product.
[0019] By adopting the above technical solution, the hydrogen bonds and hydrophobic interactions within the black soybean globulin molecules are partially broken due to the use of a weakly alkaline environment, and the pH value is adjusted back to neutral after extraction. Therefore, the dissolution rate of protein in the aqueous phase is improved and the risk of alkaline degradation is eliminated, ensuring that the extract contains a constant proportion of soluble solids.
[0020] Preferably, the Polygonatum polysaccharide extract is prepared by the following steps: Polygonatum powder (steamed and dried nine times) is passed through a 40-mesh sieve and added to softened water at a mass-to-volume ratio of 1:10-1:20 g / mL. The mixture is then refluxed at 80-90℃ for 1.5-2.5 hours. The extract is coarsely filtered while hot to remove residue, and the filtrate is collected. The filtrate is concentrated to one-third of its original volume at 60℃. After cooling to room temperature, anhydrous ethanol is added with stirring until the volume fraction reaches 70%-80%. The mixture is allowed to stand at 4℃ for 12 hours for alcohol precipitation. It is then centrifuged at 6000 r / min for 15 minutes, and the bottom precipitate is collected and dried at 50℃ to constant weight to obtain crude Polygonatum polysaccharide. A quantitative amount of crude Polygonatum polysaccharide is weighed and dissolved in softened water to prepare a Polygonatum polysaccharide extract with a polysaccharide mass concentration of 40-60 mg / mL.
[0021] By adopting the above technical solution, high-purity Polygonatum polysaccharide is obtained by using high-temperature hot water reflux to break down the cell wall barrier of Polygonatum sibiricum and using high-concentration ethanol to reduce the solubility of polysaccharide and precipitate it to remove water-soluble impurities. This allows the purified polysaccharide to provide additional rheological viscosity in the formulation and, in conjunction with sodium alginate, enhance the water-holding capacity of the aqueous system.
[0022] Secondly, the present invention provides a method for preparing a dietary therapy formula for a kidney-tonifying and hair-darkening beverage, which adopts the following technical solution:
[0023] A method for preparing a kidney-tonifying and hair-darkening beverage includes the following steps:
[0024] Step 1, Aqueous phase preparation: Heat a portion of softened water to 65-70℃, and slowly add sodium alginate, sodium hexametaphosphate, potassium citrate monohydrate and dipotassium glycyrrhizate while stirring. Continue stirring until completely dissolved and hydrated to obtain a colloidal aqueous phase matrix.
[0025] Step 2, Material compounding: Add black bean protein extract, polygonatum polysaccharide extract and mulberry concentrated juice to the colloidal aqueous matrix in sequence, stir and mix evenly, and then add the remaining softened water;
[0026] Step 3, High-shear emulsification: Maintain the temperature of the mixture at 60-70℃, add sodium stearoyl lactylate and cold-pressed black sesame oil, and use a high-shear emulsifier for shear dispersion to form a primary oil-in-water crude emulsion;
[0027] Step 4, High-pressure homogenization: The crude emulsion is pumped into a high-pressure homogenizer for secondary homogenization, which refines the fat globule size through cavitation effect and shear force.
[0028] Step 5, Sterilization and Filling: The homogenized liquid is pumped into an ultra-high temperature instantaneous sterilization system for sterilization, cooled, and then sealed and filled in a sterile environment to obtain the finished product.
[0029] By adopting the above technical solution, and by using specific time-series physical processing methods and rheological engineering methods to combine macromolecular polymer hydration, multiphase media emulsification and mechanical jet pulverization, a uniform multiphase fluid product that can resist gravity phase separation for a long time is obtained, and the transformation from dispersed primary materials to the micro-state of forming a stable network structure is successfully completed.
[0030] Preferably, in step 2, black bean protein extract, polygonatum polysaccharide extract and mulberry concentrate are added to the colloidal aqueous matrix in sequence, so that the black bean protein extract first enters the colloidal aqueous matrix to form physical encapsulation, and then the acidic mulberry concentrate is mixed in.
[0031] By adopting the above technical solution, the staggered feeding logic of pre-protein feeding and post-acid intervention allows black soybean protein molecules to bind with the sodium alginate hydration layer before contacting free protons. Therefore, the dual effect of pre-prepared buffer matrix and embedded hydration layer weakens the acid impact, avoiding the rapid denaturation of protein near the isoelectric point.
[0032] Preferably, step 3 is implemented as follows: in a high-shear emulsifier, the shearing speed is set to 9000-11000 r / min, and the shearing and dispersion is continued for 5-10 minutes to break up the oil phase droplets and make the emulsifier adhere to their surface.
[0033] By adopting the above technical solution, the strong mechanical tearing force and fluid turbulence generated by high rotation speed are used to overcome the interfacial tension between the oil and water phases and to divide the continuous oil phase into discrete droplets. Therefore, the effect of promoting the rapid adsorption of sodium stearoyl lactylate molecules at the new interface is obtained, and a primary physical barrier is constructed to prevent droplet merger.
[0034] Preferably, in step 4, the high-pressure homogenization process adopts a two-stage homogenization operation with stepped pressure drop: the first-stage homogenization pressure is set to 20-30 MPa, the second-stage homogenization pressure is set to 4-6 MPa, and the homogenization temperature is controlled at 60-65℃.
[0035] By adopting the above technical solution, the oil phase droplets are further refined by the high-speed jet and cavitation explosion generated when the liquid passes through the high-pressure gap of the primary homogenizing valve. Then, the liquid enters the low-pressure secondary region where fluid reflux and rearrangement occur. Therefore, the effect of promoting the sodium alginate network to be firmly embedded in the protein boundary membrane around the droplets is achieved, which effectively reduces the interfacial free energy of the newly formed interface and prevents the secondary aggregation of fine droplets.
[0036] Preferably, in step 5, the parameters of the ultra-high temperature instantaneous sterilization process are: sterilization at 135-137℃ for 4-6 seconds, followed by cooling to below 25℃.
[0037] By adopting the above technical solution, the lethal value sufficient to kill pathogenic bacteria and heat-resistant spores is provided in a very short time, the heat treatment time is shortened and the degree of heat denaturation is reduced. Therefore, the effect of achieving commercial sterility standards while completely preserving the color and functional components of the finished product is achieved.
[0038] This invention provides a dietary therapy formula for a kidney-tonifying and hair-darkening beverage and its preparation method. It has the following beneficial effects:
[0039] 1. This invention constructs a composite colloidal aqueous phase using a specific ratio of sodium alginate, sodium hexametaphosphate, and potassium citrate monohydrate, and specifies the addition sequence of black bean protein before acidic mulberry juice. This technical solution utilizes the proton buffering capacity of citrate ions and the steric hindrance of the sodium alginate polymer network to block direct contact between free hydrogen ions and the protein surface. This effectively avoids irreversible aggregation and precipitation of black bean plant protein upon contact with acidic fruit juice due to the charge dropping to the isoelectric point, and stably controls the pH range of the system within 0.15.
[0040] 2. This invention employs a two-stage high-pressure homogenization process using sodium stearoyl lactylate combined with a stepped pressure reduction to process cold-pressed black sesame oil. This operation utilizes the jet and cavitation effects generated by the high-pressure homogenizer to refine the dispersed phase droplets to between 0.3 and 1 micrometer, promoting rapid adsorption of emulsifier molecules at the nascent oil-water interface and reducing interfacial free energy. The refined micro-droplet size, combined with the viscosity support of the colloidal continuous phase, provides sufficient Brownian motion capability to resist gravity, thereby eliminating the stratification phenomenon of fat floating and water separation during long-term storage. Attached Figure Description
[0041] Figure 1 The figures show a comparison of particle size distribution and polydispersity characteristics of the embodiments and comparative samples of the present invention under dynamic laser scattering tests; wherein, (a) is a comparison of the average particle size test results, and (b) is a comparison of the polydispersity index (PDI) test results.
[0042] Figure 2 The diagram shows the zeta potential distribution curves of the sample solutions prepared according to the various process formulations in this embodiment of the invention.
[0043] Figure 3 The figures are comparison charts of apparent viscosity and rheological properties of various process formulation systems under steady-state rheological measurement conditions in the embodiments of the present invention; wherein, (a) is a comparison chart of rheological response scatter plot fitting curves of apparent viscosity as a function of shear rate, and (b) is a comparison chart of the distribution characteristics of flow behavior index (n) of the finished products of each scheme.
[0044] Figure 4The figures are comparison charts of the acid resistance buffering and anti-settling performance of various process formulation systems in the embodiments of the present invention under extreme environmental simulation; wherein, (a) is a comparison chart of the pH value variation range (ΔpH) test results induced by the intervention of acidic fruit juice in the material compounding process, and (b) is a comparison chart of the centrifugal sedimentation rate test results of various liquid finished products under high-intensity centrifugal field.
[0045] Figure 5 The figures are comparison diagrams of phase separation and storage stability characteristics under multiple light scattering in the embodiments of the present invention; wherein, (a) is a comparison diagram of the dynamic evolution of the overall instability index (TSI) of the system during the 168-hour accelerated isothermal cycle, and (b) is a comparison diagram of the backscattered light range (ΔBS) measurement in the top region of the measuring cell.
[0046] Figure 6 The following is a comparison chart of the fluid friction dynamics evaluation of various process formulation systems in the simulated oral soft contact interface according to the embodiments of the present invention; wherein, (a) is a comparison chart of the evolution characteristics of the contact friction coefficient of each sample liquid in the full sliding speed domain (Stribeck curve), and (b) is a comparison chart of the characteristic friction coefficient extraction values of the low-speed boundary friction zone (simulating the tight pressure of the tongue surface) and the medium-speed mixed friction zone (simulating the spreading and sliding of the liquid surface) selected at a fixed point. Detailed Implementation
[0047] 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.
[0048] The acid value of cold-pressed black sesame oil is no higher than 2 mg KOH / g and the peroxide value is no higher than 0.15 g / 100g. The soluble solids content of mulberry concentrate is 25 to 30 Brix and the total acid mass fraction is 1.5% to 2.5%.
[0049] Sodium stearoyl lactylate, CAS number 25383-99-7, has the molecular formula C. 24 H 43 NaO6.
[0050] Dipotassium glycyrrhizate, CAS number 68797-35-3, has the molecular formula C0. 42 H 60 K2O 16 .
[0051] Sodium alginate (CAS No. 9005-38-3) is a linear block copolymer polymer composed of β-D-mannuronic acid and α-L-guluronic acid linked by (1,4) glycosidic bonds. Its dynamic viscosity at 20°C is not less than 200 mPa·s at a mass% aqueous solution.
[0052] Sodium hexametaphosphate, CAS number: 10124-56-8, has the molecular formula (NaPO3)6.
[0053] The molecular formula of potassium citrate monohydrate (CAS number: 6100-05-6) is K3C6H5O7·H2O.
[0054] Preparation Example 1:
[0055] This preparation example provides a method for preparing black bean protein extract in a dietary formula for a kidney-tonifying and hair-darkening beverage, including the following steps:
[0056] Non-GMO black soybeans were pulverized through a 60-mesh sieve to obtain black soybean powder. The black soybean powder was mixed with softened water at a mass-to-volume ratio of 1:10 g / mL and then pulped. A 5% sodium bicarbonate aqueous solution was added dropwise using an automated titrator to adjust the pH of the system to 8.2. The mixture was then extracted by continuous mechanical stirring in a 45℃ constant temperature water bath for 2 hours. After extraction, the mixture was centrifuged at 5000 rpm for 15 minutes, and the supernatant was collected. Then, a 5% anhydrous citric acid aqueous solution was slowly added dropwise to adjust the pH of the supernatant back to 7. Finally, the supernatant was concentrated by vacuum rotary evaporation or by adding softened water to precisely adjust the soluble solids mass fraction to 9%. The mixture was then sterilized in a 0.10 MPa autoclave at 121℃ for 15 minutes and cooled for storage to obtain the black soybean protein extract.
[0057] Preparation Example 2:
[0058] This preparation example provides a method for preparing black bean protein extract in a kidney-tonifying and hair-darkening beverage, including the following steps:
[0059] Non-GMO black soybeans were pulverized through a 60-mesh sieve to obtain black soybean powder. The black soybean powder was mixed with softened water at a mass-to-volume ratio of 1:8 g / mL and then pulped. A 5% sodium bicarbonate aqueous solution was added dropwise using an automated titrator to adjust the pH of the system to 8. The mixture was then extracted by continuous mechanical stirring in a 40℃ constant temperature water bath for 1.5 hours. After extraction, the mixture was centrifuged at 5000 rpm for 15 minutes, and the supernatant was collected. Then, a 5% anhydrous citric acid aqueous solution was slowly added dropwise to adjust the pH of the supernatant back to 7. Finally, the supernatant was concentrated by vacuum rotary evaporation or by adding softened water to precisely adjust the soluble solids mass fraction to 8%. The mixture was then sterilized in a 0.10 MPa autoclave at 121℃ for 15 minutes and cooled for storage to obtain the black soybean protein extract.
[0060] Preparation Example 3:
[0061] This preparation example provides a method for preparing black bean protein extract in a dietary formula for a kidney-tonifying and hair-darkening beverage, including the following steps:
[0062] Non-GMO black soybeans were pulverized through a 60-mesh sieve to obtain black soybean powder. The black soybean powder was mixed with softened water at a mass-to-volume ratio of 1:12 g / mL and then pulped. A 5% sodium bicarbonate aqueous solution was added dropwise using an automated titrator to adjust the pH of the system to 8.4. The mixture was then extracted by continuous mechanical stirring in a 50°C constant temperature water bath for 2.5 hours. After extraction, the mixture was centrifuged at 5000 rpm for 15 minutes, and the supernatant was collected. Then, a 5% anhydrous citric acid aqueous solution was slowly added dropwise to adjust the pH of the supernatant back to 7. Finally, the supernatant was concentrated by vacuum rotary evaporation or by adding softened water to precisely adjust the soluble solids mass fraction to 10%. The mixture was then sterilized in a 0.10 MPa autoclave at 121°C for 15 minutes and cooled for storage to obtain the black soybean protein extract.
[0063] Preparation Example 4:
[0064] This preparation example provides a method for preparing Polygonatum polysaccharide extract in a kidney-tonifying and hair-darkening beverage, including the following steps:
[0065] The nine-times-steamed and nine-times-dried Polygonatum powder was passed through a 40-mesh sieve to obtain Polygonatum powder. Softened water was added at a mass-to-volume ratio of 1:15 g / mL, and the mixture was refluxed for 2 hours under a constant temperature water bath at 85℃. After extraction, the mixture was coarsely filtered through a 200-mesh filter cloth while still hot to remove residue. The filtrate was collected and then concentrated to one-third of its original volume in a vacuum rotary evaporator at 60℃. After cooling to room temperature, anhydrous ethanol was slowly added while continuously stirring until the volume fraction of ethanol in the mixture reached 75%. The mixture was then placed in a cold storage at 4℃ for 12 hours for alcohol precipitation. After standing, the mixture was centrifuged at 6000 r / min for 15 minutes. The bottom precipitate was collected and dried at a constant temperature of 50℃ in a vacuum drying oven to obtain crude Polygonatum polysaccharide. Finally, a quantitative amount of crude Polygonatum polysaccharide was weighed and dissolved in softened water to prepare a Polygonatum polysaccharide extract with a polysaccharide mass concentration of 50 mg / mL.
[0066] Preparation Example 5:
[0067] This preparation example provides a method for preparing Polygonatum polysaccharide extract in a kidney-tonifying and hair-darkening beverage, including the following steps:
[0068] The nine-times-steamed and nine-times-dried Polygonatum powder was passed through a 40-mesh sieve to obtain Polygonatum powder. Softened water was added at a mass-to-volume ratio of 1:10 g / mL, and the mixture was refluxed for 1.5 hours under a constant temperature water bath at 80℃. After extraction, the mixture was coarsely filtered through a 200-mesh filter cloth while still hot to remove residue. The filtrate was collected and then concentrated to one-third of its original volume in a vacuum rotary evaporator at 60℃. After cooling to room temperature, anhydrous ethanol was slowly added while continuously stirring until the volume fraction of ethanol in the mixture reached 70%. The mixture was then placed in a cold storage at 4℃ for 12 hours to allow alcohol precipitation. After standing, the mixture was centrifuged at 6000 r / min for 15 minutes. The bottom precipitate was collected and dried at a constant temperature of 50℃ in a vacuum drying oven to obtain crude Polygonatum polysaccharide. Finally, a quantitative amount of crude Polygonatum polysaccharide was weighed and dissolved in softened water to prepare a Polygonatum polysaccharide extract with a polysaccharide mass concentration of 40 mg / mL.
[0069] Preparation Example 6:
[0070] This preparation example provides a method for preparing Polygonatum polysaccharide extract in a kidney-tonifying and hair-darkening beverage, including the following steps:
[0071] The nine-times-steamed and nine-times-dried Polygonatum powder was passed through a 40-mesh sieve to obtain Polygonatum powder. Softened water was added at a mass-to-volume ratio of 1:20 g / mL, and the mixture was refluxed for 2.5 hours under a constant temperature water bath at 90℃. After extraction, the mixture was coarsely filtered through a 200-mesh filter cloth while still hot to remove residue. The filtrate was collected and then concentrated to one-third of its original volume in a vacuum rotary evaporator at 60℃. After cooling to room temperature, anhydrous ethanol was slowly added while continuously stirring until the volume fraction of ethanol in the mixture reached 80%. The mixture was then placed in a cold storage at 4℃ for 12 hours for alcohol precipitation. After standing, the mixture was centrifuged at 6000 r / min for 15 minutes. The bottom precipitate was collected and dried at a constant temperature of 50℃ in a vacuum drying oven to constant weight to obtain crude Polygonatum polysaccharide. Finally, a quantitative amount of crude Polygonatum polysaccharide was weighed and dissolved in softened water to prepare a Polygonatum polysaccharide extract with a polysaccharide mass concentration of 60 mg / mL.
[0072] Example 1:
[0073] This embodiment provides a method for preparing a dietary therapy formula for a kidney-tonifying and hair-darkening beverage, including the following steps:
[0074] (1) Aqueous phase preparation: Weigh 500g of softened water and heat it to 65°C to 70°C in a jacketed kettle. Under mechanical stirring, slowly and evenly add 1.5g sodium alginate, 0.5g sodium hexametaphosphate, 1g potassium citrate monohydrate and 0.3g dipotassium glycyrrhizate. Continue stirring for 20 minutes until the solid powder is completely dissolved and hydrated to obtain a colloidal aqueous phase matrix.
[0075] (2) Material compounding: 200g of black bean protein extract prepared in Preparation Example 1, 100g of Polygonatum polysaccharide extract prepared in Preparation Example 4 and 50g of mulberry concentrated juice were added to the above colloidal aqueous phase matrix in sequence. After stirring and mixing evenly, softened water was added to make the total weight of the aqueous phase reach 1000g.
[0076] (3) High shear emulsification: The temperature of the mixture is maintained at 65°C. 2g of sodium stearoyl lactylate and 30g of black sesame cold-pressed oil are added to it. Then it is transferred to a high shear emulsifier and sheared and dispersed at a speed of 10000r / min for 8 minutes, so that the oil phase is fully broken and coated with emulsifier to form a uniform primary oil-in-water (O / W) type crude emulsion.
[0077] (4) High-pressure homogenization: The crude emulsion is pumped into a high-pressure homogenizer for two-stage homogenization. The first-stage homogenization pressure is set to 25 MPa, the second-stage homogenization pressure is set to 5 MPa, and the homogenization temperature is 60℃. Through strong cavitation effect and shear force, the fat globule particle size is refined to less than 1 μm, and an extremely stable emulsion is obtained.
[0078] (5) Sterilization and filling: The homogenized liquid is pumped into the ultra-high temperature instantaneous sterilization (UHT) system and sterilized at 135°C for 5 seconds. Then it is rapidly cooled to below 25°C and filled into sterilized composite packaging containers under aseptic conditions. The finished product is then sealed and packaged.
[0079] Example 2:
[0080] This embodiment provides a method for preparing a dietary therapy formula for a kidney-tonifying and hair-darkening beverage, including the following steps:
[0081] (1) Aqueous phase preparation: Weigh 500g of softened water and heat it to 65°C to 70°C in a jacketed kettle. Under mechanical stirring, slowly and evenly add 1g of sodium alginate, 0.3g of sodium hexametaphosphate, 0.8g of potassium citrate monohydrate and 0.2g of dipotassium glycyrrhizate. Continue stirring for 20 minutes until the solid powder is completely dissolved and hydrated to obtain a colloidal aqueous phase matrix.
[0082] (2) Material compounding: 150g of black bean protein extract prepared in Preparation Example 2, 80g of Polygonatum polysaccharide extract prepared in Preparation Example 5 and 40g of mulberry concentrated juice were added to the above colloidal aqueous phase matrix in sequence. After stirring and mixing evenly, softened water was added to make the total weight of the aqueous phase reach 1000g.
[0083] (3) High shear emulsification: The temperature of the mixture is maintained at 60°C. 1.5g of sodium stearoyl lactylate and 20g of black sesame cold-pressed oil are added to it. Then it is transferred to a high shear emulsifier and sheared and dispersed at a speed of 9000r / min for 10 minutes, so that the oil phase is fully broken and coated with emulsifier to form a uniform primary oil-in-water (O / W) type crude emulsion.
[0084] (4) High-pressure homogenization: The crude emulsion is pumped into a high-pressure homogenizer for two-stage homogenization. The first-stage homogenization pressure is set to 20 MPa, the second-stage homogenization pressure is set to 4 MPa, and the homogenization temperature is 60℃. The fat globule particle size is refined through strong cavitation effect and shear force to obtain an extremely stable emulsion.
[0085] (5) Sterilization and filling: The homogenized liquid is pumped into the ultra-high temperature instantaneous sterilization (UHT) system and sterilized at 137°C for 4 seconds. Then it is rapidly cooled to below 25°C and filled into sterilized composite packaging containers under aseptic conditions. The finished product is then sealed and packaged.
[0086] Example 3:
[0087] This embodiment provides a method for preparing a dietary therapy formula for a kidney-tonifying and hair-darkening beverage, including the following steps:
[0088] (1) Aqueous phase preparation: Weigh 500g of softened water and heat it to 65°C to 70°C in a jacketed kettle. Under mechanical stirring, slowly and evenly add 2g of sodium alginate, 0.8g of sodium hexametaphosphate, 1.2g of potassium citrate monohydrate and 0.4g of dipotassium glycyrrhizate. Continue stirring for 20 minutes until the solid powder is completely dissolved and hydrated to obtain a colloidal aqueous phase matrix.
[0089] (2) Material compounding: 250g of black bean protein extract prepared in Preparation Example 3, 120g of Polygonatum polysaccharide extract prepared in Preparation Example 6 and 60g of mulberry concentrated juice were added to the above colloidal aqueous phase matrix in sequence. After stirring and mixing evenly, softened water was added to make the total weight of the aqueous phase reach 1000g.
[0090] (3) High shear emulsification: The temperature of the mixture is maintained at 70°C. 2.5g of sodium stearoyl lactylate and 40g of black sesame cold-pressed oil are added to it. Then it is transferred to a high shear emulsifier and sheared and dispersed at a speed of 11000r / min for 5 minutes, so that the oil phase is fully broken and coated with emulsifier to form a uniform primary oil-in-water (O / W) type crude emulsion.
[0091] (4) High-pressure homogenization: The crude emulsion is pumped into a high-pressure homogenizer for two-stage homogenization. The first-stage homogenization pressure is set to 30 MPa, the second-stage homogenization pressure is set to 6 MPa, and the homogenization temperature is 65°C. The fat globule size is refined by strong cavitation effect and shear force to obtain an extremely stable emulsion.
[0092] (5) Sterilization and filling: The homogenized liquid is pumped into the ultra-high temperature instantaneous sterilization (UHT) system and sterilized at 135°C for 6 seconds. Then it is rapidly cooled to below 25°C and filled into sterilized composite packaging containers under aseptic conditions. The finished product is then sealed and packaged.
[0093] Comparative Example 1:
[0094] Compared with Example 1, the difference is that sodium hexametaphosphate and potassium citrate monohydrate were not added in step (1) aqueous phase preparation, while the rest were the same.
[0095] Comparative Example 2:
[0096] Compared with Example 1, the difference is that in step (2) material compounding, the order of adding materials is changed to first mixing the black bean protein extract and mulberry concentrate evenly, and then adding them to the colloidal aqueous matrix. The rest are the same.
[0097] Comparative Example 3:
[0098] Compared with Example 1, the difference is that sodium alginate was not added in step (1) of aqueous phase preparation, but the rest are the same.
[0099] Comparative Example 4:
[0100] Compared with Example 1, the difference is that in step (4) high-pressure homogenization, a single-stage homogenization operation is used (only the homogenization pressure is set to 25MPa, and there is no second-stage homogenization setting), while the rest are the same.
[0101] Test Example 1:
[0102] 10 mL of the liquid beverage products prepared in Examples 1 to 3, and Comparative Examples 3 and 4 were taken as test objects. The test sample was diluted appropriately with ultrapure water filtered through a 0.22 μm microporous membrane at room temperature. The dilution ratio was controlled within the range of 1:150 to 1:250 until the transmittance of the system met the sample introduction requirements of the testing instrument to eliminate the multiple scattering effect in the optical path.
[0103] The diluted test solution was slowly injected into the polystyrene sample cell that had been pre-rinsed with deionized water and placed in the detection chamber of the dynamic laser scattering (DLS) instrument. The system measurement temperature was set at 25±0.1℃ and subjected to a constant temperature equilibrium treatment for 120 seconds. Before the test, the refractive index of the solvent input into the system was 1.330, and the initial refractive index of the dispersed phase particles was preset to 1.450.
[0104] Start the measurement program, set 15 consecutive scans for each independent sample as a complete measurement cycle, set the acquisition time of a single light intensity scan signal to 10 seconds, and fix the detection scattering angle of the photomultiplier tube at 90 degrees. Repeat the measurement three times for the same sample under the same sample preparation conditions to obtain effective attenuation data.
[0105] The system collects the light intensity autocorrelation function fluctuation signal from the detector, imports it into the system's built-in cumulative fitting model for background baseline subtraction and data smoothing, and finally uses software to calculate and extract the average particle size and polydispersity index (PDI) values of each system sample.
[0106] Table 1. Test results of average particle size and polydispersity index for each example and comparative sample:
[0107] Sample Name Average particle size (nm) Polydispersity Index (PDI) Example 1 403.6±12.4 0.176±0.015 Example 2 391.2±18.7 0.162±0.011 Example 3 418.7±15.3 0.198±0.014 Comparative Example 3 1302.4±45.6 0.442±0.038 Comparative Example 4 1754.9±63.8 0.518±0.052
[0108] According to Table 1 and Figure 1 The data shows that the primary emulsions and liquid products prepared in the example groups (Examples 1 to 3) exhibit highly convergent characteristics in terms of physical and thermodynamic states. Their average particle size is stably pinned at around 400 nm, and the polydispersity index (PDI) is less than 0.2. Conventional emulsion fluid processing often faces the problem of droplet reorganization caused by high surface energy. The microscopic interface morphology is easily deformed due to Brownian motion after shearing, which is fully confirmed in the test data of Comparative Example 4. Comparative Example 4, which abandons the secondary homogeneous pressure relief buffer, directly causes the torn oil phase droplets and protein particles to undergo irreversible flocculation and exclusion in the system due to the instantaneous high surface energy. This causes the interference light intensity in the entire measurement volume to decrease sharply, which is reflected in the macroscopic data as a particle size exceeding 1750 nm and a sudden increase in the PDI, which is labeled as a highly polydisperse state.
[0109] Intervention targeting the material reaction mechanism also dominated the tension distribution at the phase interface. Comparative Example 3, with its sodium alginate hydration coating removed, still experienced a surge in free phase particle size to over 1300 nm despite undergoing consistent high-pressure mechanical shearing treatment. Lacking the interpenetrating network of linear block copolymers, the free plant proteins completely lost the steric hindrance provided by the colloidal barrier when facing unavoidable thermal shock. This lack of microscopic steric hindrance meant that suspended phase particles had almost no repulsive margin against aggregation as contact frequency increased. This scheme remodeled the primary fat globules encapsulated by the complex salt and polysaccharide molecular chains of the material using a two-stage stepped pressure drop method. The stepped pressure mechanical force forcibly embedded the colloidal coating network into the broken oil droplets and protein interfacial membrane, locking the droplet re-aggregation channel before the shear flow field returned to atmospheric pressure. These physical orientation indicators directly traced back and confirmed the reliability of the system's anti-demulsification mechanism.
[0110] Test Example 2:
[0111] Liquid beverages prepared in Examples 1, 2, and 3, as well as Comparative Examples 1 and 3, were used as experimental subjects. Using a pipette, 2 mL of each liquid beverage was transferred to an Erlenmeyer flask containing 98 mL of deionized water. The mixture was slowly shaken at room temperature to ensure homogeneity, diluting the sample system to one-fiftieth of its original concentration to maintain suitable optical transparency for detection and reduce interference from multiple light scattering caused by the high-concentration dispersed phase on the particle electrophoretic mobility signal.
[0112] Rinse the internal flow channels and electrode areas of the folded capillary sample cell (DTS1070) multiple times with ultrapure water. Draw up the diluted dispersion to be tested with a disposable syringe and slowly inject the liquid into one end of the electrode cell. During the operation, gently pull the syringe core and tap the cell wall to force out the tiny air bubbles trapped in the detection optical path area. After confirming that the capillary U-shaped tube is filled with a continuous column of liquid without air bubbles, insert the sample cell into the measurement chamber of the Zeta potentiometer.
[0113] In the control interface of the instrument's supporting system, the ambient temperature of the measurement chamber was set to 25℃ and allowed to preheat for 180 seconds. In the medium parameter setting panel, the dielectric constant of the dispersion medium was set to 78.5, and the viscosity was confirmed to be 0.8872 cP. The system automatically matched an electric field strength of 20V to 50V based on the conductivity of the dispersion at this time, and used phase analysis light scattering technology to capture the frequency shift signal of the droplets moving towards the opposite electrode after the voltage was applied.
[0114] Using the Smoluchowski theoretical model, a mathematical conversion relationship between the electrophoretic mobility of the test sample solution and the surface potential of the system was established. Three independent measurements were performed for each test number. Each measurement program included 12 to 25 sub-loop runs automatically adjusted according to the signal-to-noise ratio. After the measurement, the mean and standard deviation of the Zeta potential obtained from the instrument processing were exported.
[0115] Table 2. Zeta potential test results for each example and comparative sample:
[0116] Sample Name Zeta potential test value (mV) Example 1 -41.7±2.6 Example 2 -37.9±1.8 Example 3 -46.2±3.1 Comparative Example 1 -14.3±4.5 Comparative Example 3 -22.8±3.4
[0117] According to Table 2 and Figure 2 The data shows that the Zeta potential of the system in the example group was stable in the range of -37mV to -47mV, establishing the effectiveness of the anti-agglomeration mechanism of the system from the electrochemical interface. In colloidal rheology research, there is often an empirical benchmark: when the absolute value of the electrostatic charge of a liquid-phase dispersion system exceeds 30mV, the electric double layer of the sliding surface of the microparticle framework will generate a repulsive energy barrier sufficient to resist van der Waals forces. Plant-based protein beverages often face the challenge of microparticle aggregation due to environmental pH fluctuations during the industrial formulation stage, especially after the addition of total acid media such as fruit juice extracts. Multiple electrostatic shielding can push the solution potential to near the isoelectric point of the protein, leading to phase separation. The sudden change in the data of Comparative Example 1 confirmed the previously proposed risk expectations. Because the chelating buffer network maintained by sodium hexametaphosphate and potassium citrate monohydrate was stripped off, the test potential dropped sharply to -14.3mV. This indicates that free hydrogen ions and a small amount of divalent cations neutralized most of the free negative charge of black bean globulin at the moment of mixing with the liquid. The stripped charge coating directly induced the formation of visible flocculent material in the milk wall.
[0118] The difficulty in masking demulsification despite simply increasing the proportion of surfactant in conventional formulations has been a persistent challenge in process development. The test results of Comparative Example 3 confirm this mechanical deficiency: the lack of long-chain sodium alginate macromolecules means that the polar group arrangement provided by limited small-molecule emulsifiers cannot effectively anchor the liquid-phase interface. In the example system, during the high-temperature, high-pressure homogenization process, the sheared and torn fine protein and oil droplet surfaces rapidly adsorbed fully hydrated and ionized sodium alginate carboxyl segments. This reconstructed anionic layer contributed the vast majority of the negative potential increment in macroscopic measurements, artificially widening the repulsive distance during particle collisions to cope with thermodynamic oscillations during storage, and completely reversing the sedimentation phenomenon caused by the fragile interfacial film in acidic fruit-flavored protein beverages.
[0119] Test Example 3:
[0120] The liquid beverage products prepared in Examples 1, 2, 3, and Comparative Example 3 were selected as the test objects for rheological properties. 150 mL of each sample was measured and placed in a sealed glass sampling bottle, then placed in a constant temperature water bath set at 25.0 ± 0.1 °C for 45 minutes for equilibration pretreatment to eliminate the interference of the previous handling and shaking process and temperature fluctuations on the entanglement state of macromolecular chains and the colloidal rheological history within the system.
[0121] Turn on the rotational rheometer main unit and its connected air compression system, and assemble the coaxial cylindrical test rotor (such as CC27 specification). Slowly pour the pretreated single sample along the inner wall of the test cup to the mark line position, lower the rotor to immerse it in the liquid phase, close the temperature-controlled windproof cover, and let it stand for 300 seconds after the system temperature stabilizes. This allows the sample to complete the thermal stress release and internal structure reconstruction in the measurement gap, avoiding the influence of residual stress generated by sample shearing on the deviation of the initial low shear data.
[0122] A steady-state rheological (flow scan) test sequence was established in the rheological testing software, and a continuously increasing shear field was applied to the rotor. The shear rate scan range was set to 1 s. -1 up to 100s -1 A logarithmic distribution pattern was used to collect 20 data points at equal intervals within this interval, with a dwell time of 15 seconds for each shear gradient to ensure that the instrument detects steady-state torque.
[0123] Record the shear stress and apparent viscosity constant of the system at different shear rates. After outputting the test data, the shear rate is truncated to 10 s. -1 (Simulating low-shear conditions in material pipeline transportation) and 100s -1 (Simulating high-shear conditions during oral swallowing) The apparent viscosity values at two nodes were combined with the Ostwald-deWaele power-law model for non-Newtonian fluids to obtain the flow behavior index (n) for each group of samples.
[0124] Table 3. Test results of apparent viscosity and flow behavior characteristics of each example and comparative system:
[0125] Sample Name <![CDATA[Apparent viscosity @ 10 s -1 (mPa·s)]]> <![CDATA[Apparent viscosity @ 100 s -1 (mPa·s)]]> Mobility Behavior Index (n) Example 1 18.24±0.35 11.41±0.18 0.735±0.012 Example 2 16.58±0.41 10.92±0.22 0.771±0.019 Example 3 20.37±0.52 12.56±0.27 0.686±0.015 Comparative Example 3 4.15±0.11 3.82±0.09 0.963±0.006
[0126] According to Table 3 and Figure 3 The data shows that the example groups (Examples 1 to 3) are in a low shear field (10s) -1 The apparent viscosity of the system under the given conditions remained in the range of 16.58 to 20.37 mPa·s, and increased with shear rate to 100 s⁻¹. -1The internal friction resistance showed a significant nonlinear decline, and the corresponding flow behavior index (n) converged between 0.686 and 0.771, which, according to the rheological definition, confirms that the compound beverage has typical pseudoplastic non-Newtonian fluid characteristics. In this type of plant-based fluid engineering with high nutrient content, creating appropriate steric hindrance through polysaccharide matrix has always been the core means to prevent the sedimentation of solid particles. After the sodium alginate molecular chains are fully expanded in the aqueous phase, the originally free black bean globulin and the homogenized micro fat globules are trapped in a weak gel structure network maintained by hydrogen bonds and van der Waals forces. This physical entanglement gives the fluid a high zero-shear viscosity when it is stationary or transported at low speed in the pipeline, thereby dragging and inhibiting the relative slippage tendency of the dispersed phase under the gravitational field. Once the beverage enters the oral control state for artificial swallowing and undergoes high shear, the three-dimensional entanglement nodes are rapidly destroyed and the molecular groups are oriented in accordance with the flow field. The rapid decrease in apparent viscosity gives the product a refreshing and non-sticky sensory experience.
[0127] The mechanical collapse after removing this core macromolecular framework is clearly demonstrated in the data feedback of Comparative Example 3. The fluid in Comparative Example 3, without the addition of sodium alginate as a protective matrix, consistently exhibited viscosity readings hovering around an extremely low 3.8 to 4.3 mPa·s under both low and high shear conditions, with a flow constant of 0.963 almost reaching the limit of a perfect Newtonian fluid (n=1). The interior of the prepared liquid, lacking the resistance of the interphase network, resembled a loose, suspended phase without skeletal support. This environment, approaching the rheological properties of pure water, was utterly incapable of resisting the collision and aggregation of droplets due to Brownian motion during storage and transportation. The sharp drop in macroscopic data further confirms that simply relying on surfactant modification of tension, without viscous damping intervention, cannot kinetically block the inevitable water separation and stratification path that the plant protein compound system will undergo during long shelf life. This precisely underscores the necessity of establishing a multi-dimensional spatial steric barrier in the aqueous polysaccharide pregel process of this invention.
[0128] Test Example 4:
[0129] Semi-finished products and final liquid beverages from the material compounding stage of Examples 1, 2, and 3, as well as Comparative Examples 1 and 2, were extracted as test objects to evaluate the acid buffering performance and anti-flocculation effect of the system. The initial pH of the black bean protein extract mixed with the aqueous matrix was measured using a precision pH meter (accuracy 0.01) calibrated with a standard buffer solution. The final pH value of the system after adding acidic mulberry concentrate and stirring continuously for 3 minutes was accurately recorded. The pH range (ΔpH) caused by the addition of acidic external materials was obtained. (For Comparative Example 2, the initial pH of the black bean protein extract and the final pH value after adding acidic mulberry concentrate and stirring continuously for 3 minutes were measured to obtain the pH range).
[0130] Take 50 mL polycarbonate centrifuge tubes that have been dried to constant weight at 105 °C and calibrate their mass on an analytical balance. Use a pipette to transfer 30 mL of the final liquid product from each group into the centrifuge tube, seal the cap, and weigh again to calculate the accurate net mass of the initial sample solution in the tube.
[0131] Centrifuge tubes containing samples were symmetrically placed into the rotor chamber of a high-speed refrigerated centrifuge. The centrifuge operating parameters were set to a relative centrifugal force (RCF) of 4500 × g, and the ambient temperature of the test chamber was maintained at 20°C. The centrifugation was carried out at a constant speed for 25 minutes. After the centrifugation program was terminated and the rotor had completely stopped, the centrifuge tubes were removed very slowly to prevent secondary suspension and disturbance of the sediment at the bottom.
[0132] Pour out the supernatant and suspended emulsion from the centrifuge tube, and carefully blot away any remaining droplets adhering to the inner wall of the tube with filter paper. Transfer the centrifuge tube containing the compacted precipitate at the bottom into a 105°C electric heating drying oven for open-top drying. After 4 hours of constant temperature evaporation of free moisture, transfer it to a desiccator to cool to room temperature and weigh it. Repeat the drying process for 1 hour until the difference in mass is less than 0.5 mg, which is considered constant weight. Calculate the centrifugation sedimentation rate for each sample based on the ratio of the net mass of the anhydrous precipitate at the bottom to the total mass of the injected sample solution.
[0133] Table 4. Results of pH range and centrifugal sedimentation rate before and after compounding in each example and comparative system:
[0134] Sample Name pH range before and after compounding (ΔpH) Centrifugal sedimentation rate (%) Example 1 0.12±0.03 1.34±0.15 Example 2 0.13±0.04 1.58±0.18 Example 3 0.11±0.05 1.25±0.12 Comparative Example 1 1.84±0.12 14.62±0.85 Comparative Example 2 0.14±0.06 11.23±0.67
[0135] According to Table 4 and Figure 4 The data shows that the pH difference in the example groups (Examples 1 to 3) before and after the addition of acidic fruit juice to the material system was strictly suppressed to within 0.15, and the final product's centrifugal sedimentation rate remained at an extremely low level of less than 1.6%. This macroscopic physicochemical indicator confirms that the composite pairing system possesses excellent acid buffering and anti-denaturation capabilities in resisting media shock. In the industrial manufacturing of plant-derived protein-based beverages, high-molecular-weight proteins often lose their microscopic electrostatic repulsion due to the disappearance of their surface net charge when approaching their isoelectric point (pH range around 4.5), resulting in frequent irreversible isoelectric point flocculation and coarse precipitation. In Comparative Example 1, where sodium hexametaphosphate and potassium citrate monohydrate were completely removed, the pH difference was drastically amplified to 1.84 upon the addition of mulberry concentrate because the system could not absorb the surge of hydrogen ions, accompanied by a coarse precipitate precipitation as high as 14.62%. This directly exposes the extreme vulnerability of unprotected free protein systems to external acid shocks. The lack of a chelating buffer salt network even allows trace amounts of divalent metal cations carried by the raw materials to roam freely, further acting as catalytic bridges in the process of protein and peptide salting out and cross-linking.
[0136] Microscopic interventions in the process implementation path and timing also harbor decisive constraints in such complex fluid reactions. In Comparative Example 2, even though the complete range of buffer salts was retained in the ingredient list, the final centrifugal sedimentation rate still surged to an unacceptable 11.23% simply because the black bean protein liquid was mixed with the high-acid fruit juice first in the order of addition. Before the protein macromolecules in their exposed and free state were coated with the sodium alginate hydration solvent layer, they collided head-on with the acidic microenvironment of an extremely high concentration gradient. The instantaneous and uneven acidity transition broke through the self-equilibrium mechanism on the surface of amino acid residues, leading to the early formation of a large number of dense condensation nuclei. This scheme employs a rigorously defined logic of colloid-first, bottom liquid buffer, and acid-after-feeding. By driving free protein units to pre-embed in a wide-area network of dispersed phase constructed from sodium alginate, it establishes both a physical embedding thickness and a chemical buffer ion layer at the free molecular interface and the surface. The absolute suppressive effect of the aforementioned centrifugation solids content clearly verifies the feasibility of the mechanism for intercepting the precipitous degradation caused by acid denaturation.
[0137] Test Example 5:
[0138] Liquid beverage products prepared in Examples 1, 2, and 3, as well as Comparative Examples 3 and 4, were selected as test subjects for thermodynamic and storage stability evaluation. 20 mL of each test liquid sample was slowly injected into a cylindrical, flat-bottomed glass measuring cell that had been ultrasonically cleaned and dried with anhydrous ethanol. The filling height was controlled to approximately 45 mm, and the cell was sealed with a Teflon stopper. Throughout the operation, macroscopic air bubbles were avoided from being introduced into the inner wall of the measuring cell or below the liquid surface.
[0139] The surface of the measurement cell, which was wiped clean without leaving any marks, was moved into the testing chamber of the Turbiscan multiple light scattering instrument. The accelerated static aging temperature was set to 37±0.2℃ in the control software to simulate a high-temperature shelf-life environment, and the continuous scanning test cycle was set to 168 hours (7 days).
[0140] The instrument's near-infrared pulsed light source (emission wavelength 880nm) is activated, driving the optical probe to move back and forth in a step-by-step manner along the longitudinal axis of the measurement cell from bottom to top. The longitudinal resolution for acquiring single transmitted light and backscattered light signals is set to 40μm, and the scanning time interval is preset to acquire a complete spectrum once every 2 hours.
[0141] After the test procedure is completed, the dynamic change curve of backscattered light flux is captured. Using the system's embedded calculus algorithm, the total instability index (TSI) of the sample at the end of the entire test cycle (168h) is extracted. Based on the liquid column height range, the backscattered light range of the top region of the measurement cell (2mm to 10mm below the liquid surface) is independently extracted to calculate the oil aggregation or phase separation trend of the sample system under accelerated thermal exposure.
[0142] Table 5. Multiple light scattering test results of each embodiment and comparative system under accelerated aging environment:
[0143] Sample Name Overall Instability Index (TSI@168h) Backscattering range in the top region (ΔBS,%) Example 1 1.18±0.13 1.42±0.21 Example 2 1.34±0.17 1.75±0.28 Example 3 1.05±0.11 1.16±0.19 Comparative Example 3 8.92±0.63 14.53±1.18 Comparative Example 4 6.74±0.51 9.88±0.85
[0144] According to Table 5 and Figure 5 Data shows that, based on the comprehensive compounding and stepped pressure reshaping, the TSI values of the example groups (Examples 1 to 3), which measure global micro-variation, were all limited to an extremely low limit of 1.40 at the end of the 168-hour accelerated exposure cycle, and the backscattered light intensity fluctuation rate of the top coherent interface was less than 1.8%. In the fluid dynamics prediction and pilot-scale industrial evaluation specifications, there is a recognized mapping standard: liquid-phase dispersion samples under accelerated storage testing conditions with a TSI not exceeding 2 within one week can typically robustly span a six-month observation window during room-temperature shelf-life degradation. Plant fat microparticles, under the action of simple small-molecule emulsifiers, are highly susceptible to near-collision dominated by hydrophobic group exposure at high temperatures. Monitoring data from Comparative Example 3 confirms the indispensability of structural polysaccharides in blocking this thermal shock channel. The direct consequence of abandoning the construction of the sodium alginate network interpenetrating protective structure is that the system's TSI approaches the collapse point of 9. The completely open interface causes the detached oil droplets to migrate upwards as if there were no damper interference and undergo Oswald ripening, which in turn causes an asymmetrical rebound of up to 14.53% in the photon scattering intensity of the top detection area. The naked eye can already detect the precipitation of continuous milky white fat rings at the top of the measurement cell.
[0145] The collapse of thermal barrier is not the only path to phase separation; residual high surface shear potential energy will also slowly erode the emulsion interface during later storage. Compared to the incomplete composition of Comparative Example 3, Comparative Example 4, although possessing a complete polysaccharide and buffer system, still carries a large amount of unreleased surface reaction energy due to the interruption of the secondary homogenization and depressurization process, as the particles were instantly pulverized in the extremely high-pressure chamber. During the static ripening stage, these broken droplets and free proteins with excessively high free energy, in order to force themselves back to the energy ground state, disregarded the basic adsorption viscosity provided by the external emulsion and forcibly underwent structural reorganization. The longitudinal optical anomaly of the sample tube and the sudden jump in top optical flux of up to 9.88% captured by the instrument confirmed that the rearrangement of these irregular emulsion particles under stress squeezed out the water in the cross-linking gaps, causing the density difference to reverse and resulting in the floating of coarse clumps. Based on previous research into dispersion dimensions and charge boundaries, it is known that the formulation components and bi-stage mechanical shearing must form a tight compression over time. The system finally established in this invention utilizes the spatiotemporal connection between high-pressure dispersion and low-pressure shaping to tightly lock the hydrated polymer sugar chains in the interfacial gaps, completely severing the link of spontaneous thermodynamic succession within the preparation liquid.
[0146] Test Example 6:
[0147] The liquid beverage products prepared in Examples 1, 2, and 3, as well as Comparative Examples 2 and 3, were selected as test subjects for evaluating oral tribological and sensory lubrication properties. 50 mL of each group's refrigerated sample was measured and 50 mL of pre-prepared and preheated simulated artificial saliva (SSF, containing appropriate amounts of mucin and amylase, pH adjusted to 6.8) was added. The mixture was then thoroughly mixed at low to medium speed using a cantilever mechanical stirrer. The mixture was then incubated in a 37°C incubator for 10 minutes to recreate the microfluidic state of the beverage before swallowing, after dilution and enzymatic hydrolysis by saliva.
[0148] A tribological measurement module equipped with a polydimethylsiloxane (PDMS) biomimetic elastic friction pair was installed on an advanced rotational rheometer. The PDMS base and the upper spherical rotor were used to simulate the rough-soft contact interface formed by the human tongue and palate. Approximately 2 mL of the incubated sample-saliva mixture was carefully dropped onto the center of the lower elastic base. The upper spherical rotor was lowered until it made contact and excess liquid was squeezed out. The thermostatic cover was closed to stabilize the ambient temperature within the measurement gap at the standard human oral temperature of 37 ± 0.1 °C.
[0149] The rheometer system applied a constant normal load of 2N to the friction pair (the load pressure simulates the pressure exerted during normal oral swallowing and tongue scraping), and then activated continuous rotation mode, setting the sliding speed of the upper friction ball to increase logarithmically from 0.1mm / s to 1000mm / s. During the velocity gradient progression, the sensor captured the tangential friction force generated at the contact surface in real time, with the acquisition interval set to capture 10 stable signal points every half order of magnitude.
[0150] The testing terminal automatically plots the Stribeck characteristic test curves representing the evolution of fluid film lubrication in the system. Full-velocity scan data is exported, and the average friction coefficients are extracted for the extreme low-speed region of 1 mm / s (corresponding to the high-pressure boundary friction zone formed when the tongue is in close contact with the palate) and the medium-speed region of 50 mm / s (corresponding to the mixed fluid friction zone at the initial stage of swallowing).
[0151] Table 6. Test results of contact friction coefficient after mixing with simulated artificial saliva in each example and comparative system:
[0152] Sample Name Boundary friction coefficient (@1mm / s) Friction coefficient in the mixing zone (@50mm / s) Example 1 0.142±0.011 0.076±0.005 Example 2 0.158±0.009 0.081±0.007 Example 3 0.137±0.015 0.069±0.004 Comparative Example 2 0.285±0.024 0.163±0.012 Comparative Example 3 0.341±0.018 0.198±0.019
[0153] According to Table 6 and Figure 6 The data shows that the friction coefficient recorded in the example group in the boundary sliding zone (1 mm / s) simulating intense tongue and palate compression was... The coefficient remained relatively stable within the 0.13 to 0.16 layer band. When the system evolved to the medium-speed mixing friction zone (50 mm / s) where the liquid film began to take effect, this coefficient smoothly dropped to near the superlubricated baseline of 0.08. Direct compounding of soybeans and fruit juice often exposes dense, denatured protein clusters due to proton bombardment in the microenvironment. These hard particles tear the naturally occurring mucoglycoprotein membrane within the extremely narrow elastic oral cavity and directly glide across exposed epithelial sensory receptors, inducing a strong rough friction response. The system in the example maintained excellent slip characteristics even in a saliva-soaked environment, primarily due to the tight sealing of the homogeneous phase interface by a wide hydrogel layer constructed from sodium alginate. Free macromolecular chains exhibited strong adsorption, adhesion, and spreading tendencies when encountering saliva shear, transforming oil-water and solid-water friction into intra-segment friction within a highly hydrated matrix. Essentially, this constructed a low-shear-resistance barrier film at the rough, soft contact layer.
[0154] The extent of sensory degradation resulting from the loss of the aforementioned polysaccharide base masking was revealed in the comparative test results. Comparative Example 3, which removed the sodium alginate system, returned a barrier coefficient as high as 0.341 in the boundary friction test. This means that a large amount of denatured protein precipitates and flocculated fats lacking polar shell protection acted as mechanical abrasives, completely disrupting the smooth transition of the biomimetic PDMS contact surface. In real-world tasting experiences, this often leads to a persistent astringent and gritty sensation at the back of the tongue. Equally noteworthy is the surge in interfacial tension data in Comparative Example 2. Even though it balanced all theoretical components, the addition of acidic fruit pulp reversed the timing of the intervention of the protective colloid and buffer liquid, causing a sudden and intense isoelectric point dislocation collapse in the system. These recombinant hardened agglomerates, formed through irreversible hydrogen bonding, are not only substantial in size but also unable to deform along the streamlines to unload normal pressure during low-speed friction. Their persistently maintained friction constant of 0.163 at 50 mm / s indicates the destructive effect caused by the morphological distortion of free colloidal particles. This confirms that the chemical operation sequence established by this invention—pre-encapsulation for water locking followed by progressive acid resistance—not only macroscopically eliminates shelf-life stratification but also reshapes the silky smooth mechanical flow field of plant-based acidic liquid beverages at the oral ingestion point.
[0155] 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 dietary therapy formula for a kidney-tonifying and hair-darkening beverage, characterized in that, Made from the following ingredients in parts by weight: 150-250 portions of black bean protein extract; 80-120 parts of Polygonatum polysaccharide extract; 40-60 portions of concentrated mulberry juice; 20-40 parts of cold-pressed black sesame oil; Sodium stearoyl lactylate 1.5-2.5 parts; Sodium alginate 1.0-2.0 parts; Sodium hexametaphosphate 0.3-0.8 parts; Potassium citrate monohydrate 0.8-1.2 parts; Dipotassium glycyrrhizate 0.2-0.4 parts; 560-730 parts softened water; In this process, sodium alginate, sodium hexametaphosphate, and potassium citrate monohydrate form a network hydration layer in the aqueous phase, which spatially encapsulates the free protein in the black bean protein extract and the cold-pressed oil droplets from black sesame.
2. The dietary formula for a kidney-tonifying and hair-darkening beverage according to claim 1, characterized in that, The system obtained by the dietary therapy formula is an oil-in-water emulsion, and the droplets formed by the dispersion of the cold-pressed black sesame oil in the oil-in-water emulsion have an average particle size of 0.3 μm to 1 μm.
3. The dietary formula for a kidney-tonifying and hair-darkening beverage according to claim 1, characterized in that, The mass centrifugation sedimentation rate of the finished product obtained from the dietary therapy formula is 0.5% to 1.6%, and the pH difference of the dietary therapy formula before and after mixing with the mulberry concentrate is 0.05 to 0.
15.
4. The dietary formula for a kidney-tonifying and hair-darkening beverage according to claim 1, characterized in that, The black bean protein extract was prepared through the following steps: Non-GMO black soybeans were pulverized and passed through a 60-mesh sieve to obtain black soybean powder. The black soybean powder was mixed with softened water at a mass-to-volume ratio of 1:8-1:12 g / mL and then slurried. A 5% sodium bicarbonate aqueous solution was added dropwise to adjust the pH of the system to 8-8.
4. The mixture was then mechanically stirred and extracted for 1.5-2.5 hours in a constant temperature water bath at 40-50℃. After extraction, centrifuge at 5000 r / min for 15 minutes, collect the supernatant, and add 5% anhydrous citric acid aqueous solution to adjust the pH of the supernatant back to 7. The supernatant is concentrated by vacuum rotary evaporation or by adding softened water to adjust the soluble solids content to 8%-10%. The solution is then sterilized in an autoclave at 121°C for 15 minutes to obtain the final product.
5. The dietary formula for a kidney-tonifying and hair-darkening beverage according to claim 1, characterized in that, The Polygonatum polysaccharide extract was prepared by the following steps: The nine-steamed and nine-dried Polygonatum powder was passed through a 40-mesh sieve and added to softened water at a mass-to-volume ratio of 1:10-1:20 g / mL. The mixture was then refluxed at 80-90℃ for 1.5-2.5 hours. The residue was removed by coarse filtration while hot, and the filtrate was collected and concentrated to one-third of its original volume at 60℃. After cooling to room temperature, anhydrous ethanol was added with stirring until the volume fraction reached 70%-80%. The mixture was allowed to stand at 4°C for 12 hours for alcohol precipitation. After centrifugation at 6000 r / min for 15 minutes, the bottom precipitate was collected and dried at 50°C to constant weight to obtain crude Polygonatum polysaccharide. Weigh a certain amount of crude Polygonatum polysaccharide and dissolve it in softened water to prepare a Polygonatum polysaccharide extract with a polysaccharide concentration of 40-60 mg / mL.
6. A method for preparing a kidney-tonifying and hair-darkening beverage formula, used to prepare the kidney-tonifying and hair-darkening beverage formula according to any one of claims 1-5, characterized in that, Includes the following steps: Step 1: Aqueous phase preparation: Heat a portion of softened water to 65-70℃, and slowly add sodium alginate, sodium hexametaphosphate, potassium citrate monohydrate and dipotassium glycyrrhizate while stirring. Continue stirring until completely dissolved and hydrated to obtain a colloidal aqueous phase matrix. Step 2: Material compounding: Add black bean protein extract, polygonatum polysaccharide extract and mulberry concentrated juice to the colloidal aqueous matrix in sequence, stir and mix evenly, and then add the remaining softened water; Step 3: High-shear emulsification: Maintain the temperature of the mixture at 60-70℃, add sodium stearoyl lactylate and cold-pressed black sesame oil, and use a high-shear emulsifier for shear dispersion to form a primary oil-in-water crude emulsion; Step 4: High-pressure homogenization: The crude emulsion is pumped into a high-pressure homogenizer for secondary homogenization, which refines the fat globule size through cavitation effect and shear force. Step 5: Sterilization and filling: The homogenized liquid is pumped into an ultra-high temperature instantaneous sterilization system for sterilization, cooled, and then sealed and filled in a sterile environment to obtain the finished product.
7. The method for preparing a kidney-tonifying and hair-darkening beverage according to claim 6, characterized in that, In step 2, black bean protein extract, polygonatum polysaccharide extract and mulberry concentrate are added to the colloidal aqueous matrix in sequence, so that the black bean protein extract is first physically embedded in the colloidal aqueous matrix, and then the acidic mulberry concentrate is mixed in.
8. The method for preparing a kidney-tonifying and hair-darkening beverage according to claim 6, characterized in that, The specific implementation method of step 3 is as follows: In a high-shear emulsifier, the shearing speed is set to 9000-11000 r / min, and shearing and dispersion are continued for 5-10 minutes to ensure that the oil phase is fully broken up and encapsulated by the emulsifier.
9. The method for preparing a kidney-tonifying and hair-darkening beverage according to claim 6, characterized in that, In step 4, the high-pressure homogenization process employs a two-stage homogenization operation with stepped pressure drops: The primary homogenization pressure is set to 20-30 MPa, the secondary homogenization pressure is set to 4-6 MPa, and the homogenization temperature is controlled at 60-65℃.
10. The method for preparing a kidney-tonifying and hair-darkening beverage according to claim 6, characterized in that, In step 5, the parameters of the ultra-high temperature instantaneous sterilization process are as follows: Sterilize at 135-137℃ for 4-6 seconds, then cool to below 25℃.