A compound disinfectant of Chinese herbal medicine for disinfecting livestock and poultry farm environment and a use method thereof

CN122997150APending Publication Date: 2026-10-30GUAN COUNTY AGRI & RURAL AFFAIRS BUREAU
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Patent Information

Application Number
CN202611351746.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-09-02
Publication Date
2026-10-30

AI Technical Summary

Technical Problem

[0005]针对现有技术的不足,本发明提供了一种畜禽养殖场环境消毒用中草药复方消毒液及其使用方法,解决了现有植物复方消毒液在硬水稀释时因多价金属离子引发多酚絮凝共沉淀导致杀菌效力下降的问题

Benefits of technology

[0044]1、本发明通过在微观结构中利用木质素磺酸钠的阴离子骨架对质子化的苦参碱类活性成分实施静电锚定,并在外围通过烷基多糖苷构建界面水化包裹层,切断了植物提取液中多酚组分在遭遇高硬度水源时的多齿配位途径。这种结构重塑阻断了养殖场地下水中钙、镁等多价金属离子诱发的絮凝共沉淀反应,使核心杀菌成分免受网状沉淀物的卷扫拖拽,从而在实际恶劣的硬水稀释条件下能够长期维持水相中的有效药物浓度与生物学杀灭效价。

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Abstract

The present application relates to the field of animal husbandry and disinfectant technology, and discloses a Chinese herbal medicine compound disinfectant for disinfecting the environment of livestock and poultry farms and a use method thereof, the disinfectant comprising deionized water, total alkaloid water extraction concentrate of Sophora flavescens, water extraction concentrate of Artemisia argyi, sodium lignosulfonate, alkyl polyglycoside, and aqueous citric acid solution and aqueous sodium citrate solution. In the preparation process, the alkaloid components of Sophora flavescens are protonated by using acid liquid, and the sulfonic acid groups of sodium lignosulfonate are used to implement electrostatic anchoring to construct an internal coordination network, supplemented by double feedback control of motor current and conductivity for high shear depolymerization, and a hydration wrapping layer is formed on the periphery by alkyl polyglycoside, and finally the phase solidification is completed by closed-loop control of gentle alkali increase. The present application restructures the microphase state of plant extracts, cuts off the polyphenol roll-sweeping co-precipitation caused by multivalent metal ions in high-hardness water sources, maintains the effective bactericidal concentration of the aqueous phase, and avoids the shear-induced condensation plugging problem of the high-pressure spray disinfection system.
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Description

Technical Field

[0001] This invention relates to the fields of animal husbandry, veterinary medicine, and disinfectants, specifically to a compound disinfectant made from traditional Chinese medicine for disinfecting the environment of livestock and poultry farms and its application method. Background Technology

[0002] Environmental hygiene in livestock and poultry farms is fundamental to preventing the spread of diseases and ensuring the healthy development of animal husbandry. In daily disinfection operations, although traditional chemically synthesized disinfectants have strong killing capabilities, long-term and high-frequency use can easily lead to drug resistance in pathogenic microorganisms. Furthermore, residual chemicals may irritate the respiratory mucosa of farmed animals or have a negative impact on the surrounding ecological environment. Therefore, natural herbal extracts, such as Sophora flavescens and Artemisia argyi, have gradually become the focus of research and development in the field of disinfectants due to their broad-spectrum antibacterial activity and good environmental compatibility.

[0003] However, existing herbal compound disinfectants still have significant limitations in practical applications in livestock farms. When diluted with 1000 mg / L hard water for 72 hours, the effective component retention rate of existing herbal disinfectants is less than 40%. Livestock farms usually directly draw groundwater as a dilution medium when preparing disinfectants on-site. This type of water is mostly hard water with high total hardness, rich in polyvalent metal ions such as calcium and magnesium. The plant extracts naturally contain polyphenols such as tannins and alkaloid molecules that play a core bactericidal role. These components form a cross-linked network through hydrogen bonds. When the compound extracts encounter high-hardness water, the polyvalent metal ions in the water are very likely to undergo polydentate coordination reactions with the polyphenols, generating insoluble macromolecular network precipitates. During the process of the precipitates agglomerating and settling to the bottom, they will be entrained on a large scale by the hydrogen-bonded alkaloid molecules, causing sweep co-precipitation.

[0004] On the other hand, modern large-scale livestock and poultry farms generally use high-pressure micro-mist disinfection systems for space disinfection. Existing plant extract compound preparations, without underlying structural deconstruction and recombination, have colloidal particles and large molecular clusters that are difficult to adapt to complex fluid dynamics environments. When the fluid passes through a nozzle with a micron-sized aperture under the high pressure of an industrial plunger pump, it will be subjected to rapidly increasing compressive and shear stresses, which can easily trigger shear coagulation effects in confined flow channels. Conventional plant extracts experience a flow rate decrease of more than 30% after running in a 5MPa high-pressure spray system for 72 hours, resulting in solvent removal and rapid hardening and cross-linking between polymer segments. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides a traditional Chinese medicine compound disinfectant for disinfecting livestock and poultry farm environments and its application method, which solves the problem that the bactericidal efficacy of existing plant compound disinfectants decreases when diluted in hard water due to polyphenol flocculation and co-precipitation caused by polyvalent metal ions.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] In a first aspect, the present invention provides a compound disinfectant made from traditional Chinese medicine for disinfecting the environment of livestock and poultry farms, employing the following technical solution:

[0008] A traditional Chinese medicine compound disinfectant for disinfecting livestock and poultry farm environments, comprising the following components by weight percentage:

[0009] Deionized water 35-67%; total alkali of Sophora flavescens water extract concentrate 10-20%; Artemisia argyi water extract concentrate 10-20%; sodium lignosulfonate 3-8%; alkyl polysaccharide 5-10%; citric acid aqueous solution 1-4%; sodium citrate aqueous solution 2-5%.

[0010] The disinfectant is prepared by the following steps: first, the pH of the system is adjusted to 3.8-4.2 to induce the protonation of alkaloids, then sodium lignosulfonate is added to anchor the active ingredients through electrostatic interaction, followed by the addition of alkyl polysaccharides to form a hydration coating layer, and finally the pH is gradually increased to 5.5-6.0 to solidify the structure.

[0011] Preferably, the mass percentage ratio of the components is any one of the following:

[0012] Formula 1: 52% deionized water, 15% concentrated total alkali extract of Sophora flavescens, 15% concentrated water extract of Artemisia argyi, 5% sodium lignosulfonate, and 8% alkyl polysaccharide glycosides;

[0013] Formula 2: 67% deionized water, 10% concentrated total alkali of Sophora flavescens, 10% concentrated water extract of Artemisia argyi, 3% sodium lignosulfonate, and 5% alkyl polysaccharide glycosides;

[0014] Formula 3: 35% deionized water, 20% concentrated total alkali of Sophora flavescens, 20% concentrated water extract of Artemisia argyi, 8% sodium lignosulfonate, and 10% alkyl polysaccharide.

[0015] By adopting the above technical solution, the solvation effect and interfacial tension between multiple components are balanced within the set concentration gradient range, ensuring that the diffusion charge density of the drug-loaded colloidal particles reaches the critical requirement of suspension stability, and avoiding phase separation during long-term storage.

[0016] Preferably, the solid content of the total alkali water extract concentrate of Sophora flavescens and the water extract concentrate of Artemisia argyi are both limited to 20%; and the mass concentration of the citric acid aqueous solution and the sodium citrate aqueous solution are both 20%.

[0017] Preferably, the concentrated aqueous extract of total alkali from Sophora flavescens is obtained by a specific extraction process including the following steps: adding ten times the amount of deionized water and simmering for two hours to filter out the first extract; adding eight times the amount of deionized water to the residue and simmering again for one and a half hours to filter out the second extract; combining the two extracts and then concentrating under reduced pressure at 60°C and a vacuum of -0.08 MPa.

[0018] This invention also provides a method for preparing a compound disinfectant made from traditional Chinese medicine for disinfecting the environment of livestock and poultry farms, using the following technical solution:

[0019] A method for preparing a traditional Chinese medicine compound disinfectant for disinfecting livestock and poultry farm environments includes the following sequential steps:

[0020] S1 Initial Dispersion and Forced Protonation: Deionized water, concentrated total alkaloids of Sophora flavescens and concentrated water extract of Artemisia argyi were mixed in a mixing tank, and low-speed stirring was started. Citric acid aqueous solution was added dropwise to lower the pH value of the system to squeeze out hydrogen bond acceptor sites and induce protonation and recombination of alkaloids.

[0021] S2 Heating Depolymerization and Polymer Anchoring: The reaction system is heated and kept at a constant temperature, and a pre-dissolved sodium lignosulfonate solution is continuously added dropwise. During this process, the high-speed dispersion disk in the inner ring is triggered by the sudden change feedback of the current baseline of the low-speed stirring motor to carry out network depolymerization under a high shear flow field, and the endpoint of colloidal depolymerization is determined based on online conductivity data.

[0022] S3 Cooling and Homogenization and Hydration Layer Construction: The temperature inside the reactor is lowered, alkyl polysaccharide is added and stirred and homogenized while maintaining a moderate shear rate;

[0023] S4 Closed-Loop Constant-Rate Alkali Adjustment: An online pH meter and metering pump are linked in a closed loop to limit the rate of pH increase. Sodium citrate solution is added dropwise to allow the system to solidify its structure in a gentle acid-base gradient.

[0024] S5 maturation and fine filtration: After continuous low-speed stirring and maturation, the product is filtered and filled to obtain the finished product.

[0025] By employing the above technical solution, this invention achieves the untangling and assembly of plant substrates through precise physical and chemical synergistic intervention during the preparation process. The reaction process and underlying mechanism are as follows:

[0026] In step S1, the original mixture of plant concentrate contains spontaneously cross-linked hydrogen-bonded states of polyphenols and alkaloids. Adding citric acid solution introduces a large number of free hydrogen ions into the system. These high-concentration hydrogen ions, with their small ionic radius and high thermodynamic activity, enter the mixture and replace the polyphenol hydroxyl groups as new proton donors, triggering the disintegration of the substrate network. The reaction process can be described as: [polyphenol-OH···NR3-alkaloid] + H+ → [polyphenol-OH] + [H-NR3+-alkaloid]. Through this dissociation and reconstruction process, the nitrogen-containing groups in the alkaloid molecule undergo forced protonation, transforming from a bound state attached to the polyphenol backbone into positively charged quaternary ammonium salt free ions.

[0027] In step S2, the heating operation increases the degrees of freedom of movement of the polymer chain segments. The strong anionic nature of the sodium lignin sulfonate molecular chain leads to complete ionization in the aqueous phase. After being added to the system, the negatively charged lignin sulfonate ions interact with the protonated alkaloids generated in step S1 through Coulomb forces. The electrostatic anchoring reaction is expressed as: [Lignin-SO3-] + [H-NR3+-alkaloids] → [Lignin-SO3-···H-NR3+-alkaloids]. The core bactericidal component is locked around the polymer backbone. Simultaneously, the addition of the polymer causes some dissociated polyphenols to undergo pseudoplastic aggregation, resulting in changes in the rheological parameters of the material, manifested as a sudden increase in the load current of the low-speed stirring motor. Upon detecting this feedback signal, the system triggers high-speed shearing. The high shear stress instantly tears apart the pseudoplastic clusters, releasing the internal trapped solvent and ensuring that the electrostatic anchoring reaction proceeds in a homogeneous liquid phase environment. The flattening of the online conductivity slope indicates that the consumption of free ions in the aqueous phase has reached equilibrium, meaning that the micro-charge locking process is complete.

[0028] In step S3, the cooling process reduces the thermal diffusion effect within the system. The surface of the alkaloid-containing particles within the system is occupied by the anionic polymer. Upon the addition of the nonionic alkyl polysaccharide, its long alkyl chains insert into or adsorb onto the outside of the particles via van der Waals forces, allowing numerous highly hydrophilic polysaccharide ring fragments to unfold in the aqueous phase. The dense clusters of hydroxyl groups on the polysaccharide rings capture surrounding water molecules through hydrogen bonds, constructing a rigid, stress-resistant interfacial hydration layer at the outer edge of the particles.

[0029] In step S4, sodium citrate is added to the system to raise the alkalinity to meet the stability requirements for storage and application of the finished formulation. The closed-loop system limits the addition rate and gradually raises the pH, eliminating localized acid-base oversaturation gradients within the system. This slow chemical potential change environment prevents free polyphenols from exceeding kinetic safety boundaries and undergoing large-scale hydrophobic self-polymerization, ensuring that the outer glycoside molecule layer undergoes slow conformational contraction and compaction, ultimately achieving physical phase solidification of the active ingredient.

[0030] Preferably, in step S1, the temperature of the system material is controlled at 20-30℃, and the apparent shear rate is set to 100-150 s. -1 Furthermore, the pH value of the system is adjusted and stabilized between 3.8 and 4.2 by adding citric acid aqueous solution dropwise, and the effect is maintained for 20-30 minutes.

[0031] By adopting the above technical solution, a temperature range was set to balance the protonation conversion efficiency and the thermal stability of the active molecular structure under acidic conditions; the pH value was clamped in a narrow band of 3.8-4.2, providing ample competitive advantage for hydrogen ion acceptors, while blocking the side reaction of glycoside hydrolysis induced by low acidity and alkalinity.

[0032] Preferably, the specific depolymerization process in step S2 is implemented as follows: the material is heated to 60-70℃; sodium lignosulfonate is pre-dissolved in deionized water and added dropwise at a constant rate over 20-30 minutes; the current of the low-speed stirring motor is monitored in real time, and when the current value increases by more than 30% compared to the baseline before addition, a high-speed dispersion disk with a shear rate of 600-800s⁻¹ is triggered to run for 3-5 minutes, and automatically shut off when the current drops back to within ±5% of the baseline; the online conductivity data after temperature compensation is continuously recorded, and the heating source is cut off when the relative decrease rate of conductivity is less than 2.0% over 10-15 minutes.

[0033] By adopting the above technical solutions, a dual process control model based on the linkage of rheological parameters (current) and electrochemical parameters (conductivity) is constructed. The current threshold triggering mechanism ensures that the equipment only starts high-energy mechanical work when the internal clusters form substantial fluid hindrance; the conductivity slope determination mechanism overcomes the reaction endpoint blind zone caused by traditional timed heating processes, effectively preventing secondary demulsification and stratification of colloids caused by excessive shearing and thermal disturbance.

[0034] Preferably, in step S3, the cooling target is set at 30-40°C, and the alkyl polysaccharide is cooled to within 150-200 seconds. -1 Stir and homogenize at a shear rate for 15-20 minutes; in step S4, the pH increase rate is controlled at 0.1-0.2 pH units / minute. When the pH value of the system slowly rises and stabilizes at the target threshold of 5.5-6.0, stop adding sodium citrate solution.

[0035] By employing the above technical solutions, matching specific cooling gradients and shear flow fields facilitates the orderly and directional distribution of glycoside molecules. Controlling the slow alkali gradient suppresses the surge in particle collision frequency, preventing bridging and agglomeration between particles.

[0036] Secondly, this invention provides a method for using a compound disinfectant made from traditional Chinese medicine for disinfecting livestock and poultry farm environments, employing the following technical solution:

[0037] A method for using a traditional Chinese medicine compound disinfectant for disinfecting the environment of livestock and poultry farms includes the following steps:

[0038] The traditional Chinese medicine compound disinfectant was mixed with the groundwater medium in the breeding area at a volume ratio of 1:300 to prepare a diluted working stock solution.

[0039] The diluted working mother liquor is pumped into a high-pressure spray circuit equipped with a plunger pump, which forces the working pressure in the pipeline system to be maintained at 5.0 MPa. The end is applied to the aquaculture environment through a micro-mist nozzle with a nominal orifice diameter of 50 μm to avoid the shear coagulation effect in the confined flow channel and maintain continuous flow.

[0040] By employing the above technical solution, when fluid enters the extremely narrowed microporous channel driven by an industrial plunger pump, it will be subjected to a sharp increase in normal compressive stress and tangential stress on the pipe wall. Compound formulations lacking anti-deformation design, under this high hydraulic load, experience solvent removal and rapid hardening cross-linking between polymer segments, leading to blockage. The agent prepared using the process controlled in this application, after dilution, contains colloidal microparticles covered by a high-viscosity nano-hydration layer formed by polysaccharide fragments. This structural unit provides extremely low-resistance lubrication protection for the fluid traversing the micro-space, enabling the active ingredient to undergo adaptive slip deformation under the dual constraints of a 5.0 MPa mechanical force and a 50 μm physical pore size. This avoids the mechanical trapping and accumulation phenomenon derived from shear coagulation, ensuring that the absolute flow rate of the pipeline maintains a flat evolution and guaranteeing the smooth operation of the industrial disinfection system.

[0041] Preferably, the groundwater medium in the aquaculture site is extremely hard water that is attacked by polyvalent metal ions and has a total hardness of no more than 1000 mg / L (calculated as calcium carbonate); the diluted working mother liquor, after standing in the above-mentioned hard water medium for 72 hours, has a liquid phase turbidity of no more than 7.9 NTU and a mass retention rate of matrine in the aqueous phase of more than 90%.

[0042] By employing the above technical solutions, the resistance of the formulation's internal deconstruction and encapsulation system to real-world harsh application environments was confirmed from two dimensions: physical phase characterization and chemical component quantification. Under continuous attack from multivalent metal cations for over three days, the macroscopically suspended fluid maintained optical clarity, and the free bactericidal substances avoided co-loss with gravity sediments, meeting the practical application requirement of non-degradation during a long storage period after on-site preparation.

[0043] This invention provides a traditional Chinese medicine compound disinfectant for disinfecting livestock and poultry farm environments and its application method. It has the following beneficial effects:

[0044] 1. This invention utilizes the anionic framework of sodium lignosulfonate in the microstructure to electrostatically anchor protonated matrine-like active ingredients, and constructs an interfacial hydration coating layer using alkyl polysaccharides, thereby interrupting the multidentate coordination pathway of polyphenolic components in plant extracts when encountering high-hardness water. This structural reshaping blocks the flocculation and co-precipitation reactions induced by calcium, magnesium, and other polyvalent metal ions in groundwater at aquaculture sites, preventing the core bactericidal components from being swept away by network precipitates. This allows for the long-term maintenance of effective drug concentration and biological bactericidal potency in the aqueous phase even under harsh hard water dilution conditions.

[0045] 2. This invention introduces a high-shear dynamic depolymerization process based on dual feedback of motor load current and online conductivity, eliminating pseudoplastic clusters in the plant substrate liquid that easily induce rheological hindrance. Simultaneously, the high-viscosity hydration layer formed around the particles significantly reduces the interfacial resistance of the fluid. When the diluted solution passes through micron-sized nozzles driven by an industrial high-pressure plunger pump, the effective particle structure within the system can undergo adaptive deformation and slippage, avoiding the shear coagulation and pore wall hardening phenomena that easily occur in traditional plant compound preparations under extreme flow field pressure, thus ensuring the continuous and unobstructed flow of modern automated micro-mist disinfection pipelines.

[0046] 3. This invention employs a feedback control mechanism involving a closed-loop linkage between an online pH meter and a metering pump during the molding stage. This strictly limits the rate of alkalinity recovery within a gentle quantitative gradient, preventing localized oversaturation of the reaction space. This smooth transition of chemical potential effectively inhibits the large-scale hydrophobic self-polymerization of free polyphenols beyond the kinetic boundary caused by environmental abrupt changes. It ensures the slow conformational contraction and compaction of surfactant molecules around the colloid, achieving complete physical solidification of the active drug-loaded structure and significantly improving the finished formulation's resistance to stratification and degradation during long-term storage. Attached Figure Description

[0047] Figure 1 This is a schematic diagram illustrating the dynamic conductivity during the preparation process of the present invention.

[0048] Figure 2 This is a schematic diagram of the rheology and dynamic response of the motor current during the preparation process of the present invention;

[0049] Figure 3 This is a schematic diagram illustrating the evolution of hydrated particle size distribution according to the present invention;

[0050] Figure 4 This is a schematic diagram illustrating the extreme high hardness water quality tolerance and phase stability of the present invention;

[0051] Figure 5 This is a schematic diagram illustrating the retention rate of effective components after extreme water quality aging according to the present invention.

[0052] Figure 6 This is a schematic diagram simulating the attenuation rate of the automated micro-mist nozzle during continuous operation according to the present invention;

[0053] Figure 7 This is a dumbbell diagram showing the attenuation of the killing efficacy of each system against the target strain after aging in extremely hard water according to the present invention. Detailed Implementation

[0054] The technical solutions in the embodiments of the present invention will be clearly and completely described below 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.

[0055] 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.

[0056] Sodium lignosulfonate has the CAS number 8061-51-6. This compound is an anionic polymer with a cross-linked structure of sulfonic acid groups and phenolic hydroxyl groups. Its weight-average molecular weight ranges from 8,000 to 12,000, and its degree of sulfonation ranges from 1.2 mmol / g to 2.0 mmol / g.

[0057] The CAS number of the alkyl polysaccharide is 68515-73-1. This compound is a nonionic surfactant. The carbon chain length of its hydrophobic alkyl group is limited to the range of C8 to C10, and the average degree of polymerization of its hydrophilic sugar unit is limited to the range of 1.3 to 1.5. The solid content of the commercially available liquid product is 50%.

[0058] Citric acid (CAS No. 77-92-9), sodium citrate (CAS No. 6132-04-3), polysorbate 80 (CAS No. 9005-65-6), and disodium ethylenediaminetetraacetate (CAS No. 6381-92-6) are all commercially available compounds with well-defined chemical structures.

[0059] Deionized water is commercially available or can be prepared in a conventional manner, and its conductivity is less than or equal to 0.1 μS / cm.

[0060] Preparation Example 1:

[0061] This preparation example provides a method for preparing a concentrated aqueous extract of total alkaloids from Sophora flavescens, including the following steps:

[0062] Weigh out the slices of Sophora flavescens, add ten times the amount of deionized water, soak for thirty minutes, heat to boiling, and simmer for two hours. Filter out the extract. Add eight times the amount of deionized water to the dregs, and simmer again for one and a half hours. Filter out the extract. Combine the two extracts and concentrate under reduced pressure at 60 degrees Celsius and a vacuum of -0.08 MPa. Then, adjust the solid content to 20% by adding deionized water or continuing to evaporate. Cool to room temperature for later use.

[0063] Preparation Example 2:

[0064] This preparation example provides a method for preparing a concentrated aqueous extract of Artemisia argyi, including the following steps:

[0065] Weigh out the Artemisia argyi slices, add ten times the amount of deionized water, heat to boiling in an extraction tank equipped with a reflux condenser, maintain a gentle reflux for two hours, and filter out the extract; add eight times the amount of deionized water to the residue, maintain a gentle reflux for one and a half hours, and filter out the extract; combine the two extracts, concentrate under reduced pressure at 60 degrees Celsius and a vacuum of -0.08 MPa, and then precisely adjust the solid content to 20% by adding deionized water or continuing evaporation, and cool to room temperature for later use.

[0066] Example 1:

[0067] This embodiment provides a method for preparing a compound disinfectant made from traditional Chinese medicine for disinfecting the environment of livestock and poultry farms, including the following steps:

[0068] S1. 52% by mass of deionized water was added to a mixing vessel equipped with a biaxial stirring system, an online conductivity meter, and an online pH meter. Then, 15% by mass of the concentrated aqueous extract of total alkaloids from *Sophora flavescens* obtained in Preparation Example 1 and 15% by mass of the concentrated aqueous extract of *Artemisia argyi* obtained in Preparation Example 2 were pumped in sequentially at 25°C. The outer ring low-speed stirring was then turned on, and the apparent shear rate was set to 125 s. -1 Stir for 8 minutes; add 20% citric acid aqueous solution dropwise using a metering pump, and adjust and stabilize the pH of the system at 4.0 using online pH meter feedback; maintain 25℃ and stir continuously for 25 minutes.

[0069] Steam is introduced into the jacket of the reactor in S2 to heat the material to 65°C and maintain the temperature. 5% sodium lignosulfonate is pre-dissolved in 5% deionized water and continuously added dropwise to the mixing tank over 25 minutes at a constant flow rate using a metering pump. The current of the low-speed stirring motor is monitored in real time; when the current value suddenly increases by more than 30% compared to the baseline before addition, the inner high-speed dispersion disc is triggered, dispersing at a rate of 700 seconds. -1The shear rate was run for 4 minutes to depolymerize. When the motor current dropped back to within ±5% of the baseline, the high-speed dispersion disk was turned off. The online conductivity data after temperature compensation was continuously recorded. When the relative decrease rate of conductivity was less than 2.0% within 12 consecutive minutes, the steam was cut off and heating was stopped.

[0070] S3: Cooling water is introduced into the jacket to lower the temperature inside the reactor to 35°C; 8% (by mass) of alkyl polysaccharide is added, and the reaction is carried out for 175 seconds. -1 Stir and homogenize for 18 minutes at a shear rate;

[0071] S4 starts the metering pump containing a 20% sodium citrate aqueous solution. The metering pump is linked with the online pH meter in a closed loop to control the addition rate, limiting the pH rise rate of the system in the reactor to 0.15 pH units / minute. When the pH value of the system slowly rises and stabilizes at 5.8, the addition of sodium citrate solution is stopped.

[0072] S5 is held at 25°C for 75 seconds. -1 The mixture is stirred and matured at a shear rate for 40 minutes; the liquid is then pumped into a 30μm precision filter bag for filtration, and the filtrate is filled and sealed to obtain the finished herbal compound disinfectant solution.

[0073] Example 2:

[0074] This embodiment provides a method for preparing a compound disinfectant made from traditional Chinese medicine for disinfecting the environment of livestock and poultry farms, including the following steps:

[0075] S1. 67% by mass of deionized water was added to a mixing vessel equipped with a biaxial stirring system, an online conductivity meter, and an online pH meter. Then, 10% by mass of the concentrated aqueous extract of total alkaloids from *Sophora flavescens* obtained in Preparation Example 1 and 10% by mass of the concentrated aqueous extract of *Artemisia argyi* obtained in Preparation Example 2 were pumped in sequentially at 20°C. The outer ring low-speed stirring was then turned on, and the apparent shear rate was set to 100 s⁻¹. -1 Stir for 5 minutes; add 20% citric acid aqueous solution dropwise using a metering pump, and adjust and stabilize the pH of the system at 3.8 using online pH meter feedback; maintain 20℃ and continue stirring for 20 minutes.

[0076] Steam is introduced into the jacket of the reactor in S2 to heat the material to 60°C and maintain the temperature. 3% sodium lignosulfonate is pre-dissolved in 5% deionized water and continuously added dropwise to the mixing tank at a constant flow rate over 20 minutes using a metering pump. The current of the low-speed stirring motor is monitored in real time. When the current value suddenly increases by more than 30% compared to the baseline before addition, the inner high-speed dispersion disk is triggered to intervene and run at a shear rate of 600s⁻¹ for 3 minutes to depolymerize. The high-speed dispersion disk is turned off when the motor current drops back to within ±5% of the baseline. The online conductivity data after temperature compensation is continuously recorded. When the relative decrease rate of conductivity is less than 2.0% within 10 consecutive minutes, the steam is cut off to stop heating.

[0077] S3: Cooling water is introduced into the jacket to lower the temperature inside the reactor to 30°C; 5% (by mass) of alkyl polysaccharide is added, and the mixture is reacted within 150 seconds. -1 Stir and homogenize for 15 minutes at a shear rate;

[0078] S4 starts the metering pump containing a 20% sodium citrate aqueous solution. The metering pump is linked with the online pH meter in a closed loop to control the addition rate, limiting the pH rise rate of the system in the reactor to 0.1 pH units / minute. When the pH value of the system slowly rises and stabilizes at 5.5, the addition of sodium citrate solution is stopped.

[0079] S5 is kept at 20℃ for 50 seconds. -1 The mixture is stirred and matured at a shear rate for 30 minutes; the liquid is then pumped into a 10μm precision filter bag for filtration, and the filtrate is filled and sealed to obtain the finished herbal compound disinfectant solution.

[0080] Example 3:

[0081] This embodiment provides a method for preparing a compound disinfectant made from traditional Chinese medicine for disinfecting the environment of livestock and poultry farms, including the following steps:

[0082] S1. 35% by mass of deionized water was added to a mixing vessel equipped with a biaxial stirring system, an online conductivity meter, and an online pH meter. Then, 20% by mass of the concentrated aqueous extract of total alkaloids from *Sophora flavescens* obtained in Preparation Example 1 and 20% by mass of the concentrated aqueous extract of *Artemisia argyi* obtained in Preparation Example 2 were pumped in sequentially at 30°C. The outer ring low-speed stirring was then turned on, and the apparent shear rate was set to 150 s. -1 Stir for 10 minutes; add 20% citric acid aqueous solution dropwise using a metering pump, and adjust and stabilize the pH of the system at 4.2 using online pH meter feedback; maintain 30℃ and stir continuously for 30 minutes.

[0083] Steam is introduced into the jacket of the reactor in S2 to heat the material to 70°C and maintain the temperature. 8% sodium lignosulfonate is pre-dissolved in 7% deionized water and continuously added dropwise to the mixing tank over 30 minutes using a metering pump at a constant flow rate. The current of the low-speed stirring motor is monitored in real time; when the current value suddenly increases by more than 30% compared to the baseline before addition, the inner high-speed dispersion disc is triggered, dispersing at a rate of 800 seconds. -1 The shear rate is run for 5 minutes to depolymerize. When the motor current drops back to within ±5% of the baseline, the high-speed dispersion disk is turned off. The online conductivity data after temperature compensation is continuously recorded. When the relative decrease rate of conductivity is less than 2.0% within 15 consecutive minutes, the steam is cut off and heating is stopped.

[0084] S3: Cooling water is introduced into the jacket to lower the temperature inside the reactor to 40°C; 10% (by mass) of alkyl polysaccharide is added, and the mixture is reacted in 200 seconds. -1 Stir and homogenize for 20 minutes at a shear rate;

[0085] S4 starts the metering pump containing a 20% sodium citrate aqueous solution. The metering pump is linked with the online pH meter in a closed loop to control the addition rate, limiting the pH rise rate of the system in the reactor to 0.2 pH units / minute. When the pH value of the system slowly rises and stabilizes at 6.0, the addition of sodium citrate solution is stopped.

[0086] S5 was kept at 30℃ for 100 seconds. -1 The mixture is continuously stirred and matured at a shear rate for 45 minutes; the liquid is then pumped into a 50μm precision filter bag for filtration, and the filtrate is filled and sealed to obtain the finished herbal compound disinfectant solution.

[0087] Example 4:

[0088] This embodiment provides a method for preparing a compound disinfectant made from traditional Chinese medicine for disinfecting the environment of livestock and poultry farms, including the following steps:

[0089] S1. 52% by mass of deionized water was added to a mixing vessel equipped with a biaxial stirring system, an online conductivity meter, and an online pH meter. Then, 20% by mass of the concentrated aqueous extract of total alkaloids from *Sophora flavescens* obtained in Preparation Example 1 and 10% by mass of the concentrated aqueous extract of *Artemisia argyi* obtained in Preparation Example 2 were pumped in sequentially at 25°C. The outer ring low-speed stirring was then turned on, and the apparent shear rate was set to 125 s⁻¹. -1 Stir for 8 minutes; add 20% citric acid aqueous solution dropwise using a metering pump, and adjust and stabilize the pH of the system at 4.0 using online pH meter feedback; maintain 25℃ and stir continuously for 25 minutes.

[0090] Steam is introduced into the jacket of the reactor in S2 to heat the material to 65°C and maintain the temperature. 5% sodium lignosulfonate is pre-dissolved in 5% deionized water and continuously added dropwise to the mixing tank over 25 minutes at a constant flow rate using a metering pump. The current of the low-speed stirring motor is monitored in real time; when the current value suddenly increases by more than 30% compared to the baseline before addition, the inner high-speed dispersion disc is triggered, dispersing at a rate of 700 seconds. -1 The shear rate was run for 4 minutes to depolymerize. When the motor current dropped back to within ±5% of the baseline, the high-speed dispersion disk was turned off. The online conductivity data after temperature compensation was continuously recorded. When the relative decrease rate of conductivity was less than 2.0% within 12 consecutive minutes, the steam was cut off and heating was stopped.

[0091] S3: Cooling water is introduced into the jacket to lower the temperature inside the reactor to 35°C; 8% (by mass) of alkyl polysaccharide is added, and the reaction is carried out for 175 seconds. -1 Stir and homogenize for 18 minutes at a shear rate;

[0092] S4 starts the metering pump containing a 20% sodium citrate aqueous solution. The metering pump is linked with the online pH meter in a closed loop to control the addition rate, limiting the pH rise rate of the system in the reactor to 0.15 pH units / minute. When the pH value of the system slowly rises and stabilizes at 5.8, the addition of sodium citrate solution is stopped.

[0093] S5 is held at 25°C for 75 seconds. -1 The mixture is stirred and matured at a shear rate for 40 minutes; the liquid is then pumped into a 30μm precision filter bag for filtration, and the filtrate is filled and sealed to obtain the finished herbal compound disinfectant solution.

[0094] Comparative Example 1:

[0095] Compared with Example 1, the difference is that sodium lignosulfonate in step S2 is replaced with an equal amount of the conventional nonionic surfactant polysorbate 80, and all other steps are the same.

[0096] Comparative Example 2:

[0097] Compared with Example 1, the difference is that the alkyl polysaccharide in step S3 is omitted and the amount is made up with an equal amount of deionized water, while the rest are the same.

[0098] Comparative Example 3:

[0099] Compared with Example 1, the difference is that sodium lignosulfonate in step S2 and alkyl polysaccharide in step S3 are omitted and replaced with disodium ethylenediaminetetraacetate, a conventional metal chelating agent, in equal amounts. All other aspects are the same.

[0100] Comparative Example 4:

[0101] Compared with Example 1, the difference is that step-by-step dynamic process control is not performed. That is, the two extracts, sodium lignosulfonate, alkyl polysaccharide and deionized water are mixed at room temperature at one time, buffer solution is directly added to adjust the pH of the system to 5.8, and the mixture is stirred and discharged. Everything else is the same.

[0102] Comparative Example 5:

[0103] Compared with Example 1, the difference is that the acid-adjusting protonation process in step S1 is omitted, that is, the pH of the system is not adjusted to 4.0 by adding citric acid aqueous solution, and the two phases are directly mixed and then proceeded to step S2. The rest are the same.

[0104] Comparative Example 6:

[0105] Compared with Example 1, the difference lies in breaking the kinetic constraint in step S4, that is, instead of using a metering pump to control the pH increase rate, a sodium citrate aqueous solution is poured in rapidly in one go, forcibly raising the pH of the system directly from 4.0 to 5.8 within 1 minute. All other aspects are the same.

[0106] Comparative Example 7:

[0107] Compared with Example 1, the difference is that in step S2, the low-speed motor current monitoring and high-speed dispersion disc linkage intervention function are turned off, and only a low-speed constant stirring of 125s⁻¹ is maintained throughout the process, while the rest are the same.

[0108] Comparative Example 8:

[0109] Compared with Example 1, the difference is that in step S2, the relative decrease rate of conductivity is not recorded as the criterion for the thermodynamic reaction endpoint. Instead, the heating and holding time is artificially fixed at 10 minutes, and then the steam is forcibly cut off to enter the cooling step. All other steps are the same.

[0110] Test Example 1: Online conductivity kinetic monitoring during the preparation process

[0111] This test case mainly focuses on in-situ monitoring of the systems of Example 1 and Comparative Example 8, and relies on the distributed control system built into the mixing tank to extract process data non-destructively.

[0112] 1. Set the monitoring starting point as the absolute moment when the metering pump is turned on and the sodium lignosulfonate solution is started to be added in step S2, and record it as 0 minutes.

[0113] 2. By controlling the data recording log in the system background, the measured values ​​of the online four-electrode conductivity meter with built-in automatic temperature compensation algorithm are extracted every 3 minutes.

[0114] 3. Synchronously extract the relative decrease rate of conductivity over a continuous 12-minute period within the control system. This data is calculated by the system based on the relative difference between the current time and the measured maximum value within the previous 12 minutes.

[0115] 4. Continuously track and record until each group triggers a stop heating command based on its own process logic, and collect all related data sequences before termination.

[0116] Table 1. Monitoring data of online conductivity and relative decrease rate over 12 minutes.

[0117] 0 11425.3 - 11418.9 - 3 11054.1 - 11102.4 - 6 10682.7 - 10756.2 - 9 10245.9 - 10321.7 - 12 9912.4 13.24 9887.5 13.41 15 9645.8 12.74 9611.2 13.43 18 9410.2 11.91 9385.6 12.74 21 9178.5 10.41 9204.1 10.82 24 9024.1 8.96 9051.8 8.45 27 8915.6 7.57 8922.3 7.17 30 8847.2 5.98 8856.4 5.63 33 8798.5 4.14 8810.1 4.28 36 8774.1 1.59 8782.5 3.03 39 - - - -

[0118] Figure 1 This is a dynamic monitoring graph of conductivity during the preparation process of the present invention. In the graph, the black solid line and circular mark represent the conductivity evolution trajectory of Example 1 during the sodium lignosulfonate drop and subsequent heat preservation stages. The black pentagram mark is the process termination point triggered by the control system due to the decrease rate reaching the target. The dashed line and square mark represent the evolution trajectory of Comparative Example 8. The cross mark indicates the moment when the reaction of the system is forcibly cut off due to reaching the fixed heat preservation time.

[0119] According to the data in Table 1, the macroscopic conductivity of the reaction system exhibits a clear nonlinear decay trend after the introduction of sodium lignosulfonate. In the initial stage of preparation, the system contains a large number of hydrogen ions provided by citric acid and free matrine alkaloid cations dissociated from the previous protonation treatment, forming a highly conductive electrolyte background, resulting in an initial measured conductivity above 11400 μS / cm. As sodium lignosulfonate carrying strong anionic groups is continuously introduced into the reactor via a metering pump, the sulfonic acid groups on its polymer backbone exhibit high chain flexibility at high temperatures, initiating competitive electrostatic association with the protonated alkaloids in the liquid phase. Once the free ions are confined within the mesoscopic ion-pair composite structure, their free migration ability under an electric field is significantly limited, directly reflected macroscopically as a continuous decrease in the conduction current detected by the sensor.

[0120] Test Example 2: Monitoring of Rheological and Dynamic Response of Motor Current During the Fabrication Process

[0121] This test case mainly focuses on the in-situ and bypass synergistic monitoring of the evolution of rheological parameters in Example 1 and Comparative Example 7 during the addition of sodium lignosulfonate, in order to verify the engineering effectiveness of dynamic shear control intervention in overcoming the pseudoplastic gelation process of the system.

[0122] 1. Set the monitoring time starting point to the zero moment when the sodium lignosulfonate solution is started to be added to the mixing tank. Record the baseline value of the three-phase current of the outer ring low-speed stirring motor under the current state, and use the bypass circulation sampling device to obtain the apparent viscosity of the initial fluid.

[0123] 2. Relying on the distributed control system of the reactor, the measured current readings of the low-speed stirring motor are continuously recorded during the dripping and subsequent heat preservation stages. The system in Example 1 will automatically trigger the operation of the inner high-speed dispersion disk when it senses a sudden increase in current exceeding the limit, while the system in Comparative Example 7 completely disables this triggering logic and only maintains constant low-speed stirring.

[0124] 3. At critical time points, the reaction liquid sample is simultaneously extracted through the bypass pipeline and quickly introduced into the rotational rheometer. The macroscopic apparent viscosity of the sample is measured under constant test temperature and specified shear rate.

[0125] 4. Track the data throughout the entire process until the end of this stage of operation, and summarize the current and viscosity response matrices under different flow field control strategies.

[0126] Table 2 Dynamic response data of motor current and apparent viscosity during the preparation process.

[0127] 0 3.24 43.6 3.21 45.1 5 3.58 128.4 3.65 142.7 10 4.41 632.5 4.57 688.2 15 3.31 87.9 4.72 764.5 20 3.28 92.1 4.51 612.3 25 3.25 94.6 4.43 556.8 30 3.27 93.3 4.38 531.4

[0128] Figure 2 This is a rheological and motor current dynamic response monitoring diagram of the preparation process of the present invention, which includes two vertically arranged sub-graphs. Sub-graph (a) shows the transient change of the low-speed motor operating current during the addition of sodium lignosulfonate. The black solid line corresponds to Example 1 with high shear intervention logic, and the dashed line corresponds to Comparative Example 7 which relies only on low-speed stirring. Sub-graph (b) shows the fluid apparent viscosity evolution trajectory obtained synchronously with the aforementioned time nodes. The solid line corresponds to Example 1, and the dashed line corresponds to Comparative Example 7.

[0129] According to the data in Table 2, the macroscopic rheological properties of the system underwent a highly significant change in the initial stage after the introduction of the anionic polymer. Within the first 10 minutes of adding sodium lignosulfonate, the low-speed stirring motor current in both Example 1 and Comparative Example 7 climbed from a baseline of approximately 3.2 A to over 4.4 A, exceeding the safety threshold. Simultaneously, the apparent viscosity data surged dramatically from an initial state of extremely low resistance to over 600 mPa·s. This abrupt change in physical parameters originates from the localized pseudoplastic gelation behavior accompanying the macromolecular assembly process within the system. In real industrial liquid preparation environments, there are dead zones in the flow field and local concentration gradients. The high-density charged polymer, upon entering the liquid phase, readily undergoes disordered cross-linking with free protonated alkaloids and tannin fragments at high temperatures. These insufficiently stretched cross-linked networks intertwine at the mesoscale, constructing a three-dimensional gel skeleton structure with a certain yield stress, directly increasing the running resistance of the stirring impeller.

[0130] Test Example 3: Monitoring the Evolution of Particle Size and Polydispersion Index Based on Dynamic Light Scattering

[0131] This test case mainly focuses on the mesoscopic physicochemical state analysis of the finished product systems of Example 1 and Comparative Example 6. Through non-invasive light scattering technology, it verifies the real impact of deprotonation kinetic control on the construction of steric hindrance layers and self-polymerization interception.

[0132] 1. Take 5 ml of the final liquid from Example 1 and Comparative Example 6 after the maturation period, and inject them into glass containers containing 495 ml of constant temperature deionized water. Use a magnetic rotor to maintain low-frequency swirling to complete the hundredfold dilution, so as to avoid multiple light scattering interference that occurs inside the high-concentration system.

[0133] 2. Use a micropipette to draw up the diluted fluid sample and slowly inject it into the inner cavity of a clean quartz cuvette. After sealing, place it into the constant temperature test chamber of the dynamic light scattering instrument, force the ambient temperature to be locked at 25 degrees Celsius, and let it stand for 120 seconds to eliminate thermal fluctuations.

[0134] 3. Activate the instrument’s built-in non-negative least squares data inversion algorithm, and under the conditions of a fixed laser wavelength of 633 nm and a backscattering angle of 173 degrees, continuously collect the autocorrelation function of the scattered light intensity fluctuations caused by the Brownian motion of suspended particles in the sample liquid phase for 15 consecutive times.

[0135] 4. Extract the discrete matrix of hydrated particle size distribution and characteristic polydispersity index from the system output, and summarize the statistical evolution data of colloidal interface structure under different process constraints.

[0136] Table 3 Measured data on hydrated particle size distribution and percentage of scattered light intensity

[0137] 23.5 0.0 0.0 42.8 1.8 0.0 71.4 14.6 1.7 105.2 41.2 7.4 148.6 27.5 10.8 201.3 11.4 8.2 284.5 3.5 4.9 412.0 0.0 5.3 645.8 0.0 9.7 958.2 0.0 17.5 1380.4 0.0 21.2 2054.1 0.0 10.4 3120.6 0.0 2.9 4500.0 0.0 0.0

[0138] Figure 3 This is a monitoring chart of the evolution of hydrated particle size distribution in this invention. The black solid line and circular mark in the chart represent the particle size scattering light intensity distribution trajectory of the ripening endpoint product of Example 1 in the aqueous phase, and the dashed line and square mark represent the particle size distribution state of the system of Comparative Example 6 after violating the acid-base kinetic limit.

[0139] According to the data in Table 3, after the deprotonation correction phase, the evolution trajectory of the interfacial morphology of the internal colloidal particles is highly sensitive to the rate of pH change. The light scattering signal obtained in Example 1 is concentrated in an extremely narrow range, with the main hydrated particle size of the particle community converging to around 100 nm, and the instrument did not capture any statistically significant scattering peaks at the micrometer scale. This corresponds to the fact that within the process window of strictly limiting the pH increase rate to 0.15 units per minute, the nonionic surfactant molecules have sufficient physical diffusion time. Alkyl polysaccharide molecules are tightly attached to the outer interface of the nascent ion pair complex through van der Waals forces, and a dense spatial hydration layer with extremely high viscosity is constructed towards the aqueous phase by the densely arranged polyhydroxy sugar rings, completely cutting off the pathway of collisional crosslinking between adjacent particles caused by Brownian motion, resulting in an overall fluid exhibiting an extremely low polydispersity index of 0.142.

[0140] Test Example 4: Test on tolerance and phase stability to extremely high hardness water

[0141] This test case mainly focuses on the finished products of Examples 1 to 4 and Comparative Examples 1, 2, and 4, and quantitatively tracks the phase evolution under a simulated harsh groundwater dilution scenario in a farm to confirm the effectiveness of the mesoscopic reconstructed network in resisting the invasion of multivalent metal ions.

[0142] 1. Weigh anhydrous calcium chloride and magnesium chloride hexahydrate, dissolve them in deionized water at a calcium-to-magnesium ion molar ratio of 2:1, and accurately determine and adjust their total hardness to 1000 mg / L (calculated as calcium carbonate) by complexometric titration, thus using this as an artificial extreme hard water medium.

[0143] 2. Take the finished liquid from each of the above groups and add it to a standard conical flask containing 500 ml of artificial hard water at a volume ratio of 1:300. Mix the mixture for three minutes at a constant speed using a mechanical stir bar to simulate the on-site drug dilution process.

[0144] 3. Place the mixed sample solution on a light-proof experimental platform and let it stand. At absolute zero time, 24 hours and 72 hours after mixing is completed, use a micropipette to extract the sample from 2 cm below the liquid surface and inject it into the turbidity meter to read the measured turbidity value.

[0145] 4. After the turbidity test at the seventy-second hour, transfer all the remaining fluid in the conical flask, along with any visible suspended matter at the bottom, to a pre-weighed high-speed centrifuge tube and separate the solid and liquid for fifteen minutes under a centrifugal force field of 4,000 revolutions per minute.

[0146] 5. Pour off the supernatant, place the centrifuge tube in a vacuum drying oven and dry it at a constant temperature until constant weight. Calculate the mass percentage of the residual solid precipitate relative to the effective solid content in the original added drug solution.

[0147] Table 4. Turbidity evolution and final sedimentation data of different systems in extremely hard water media.

[0148] Example 1 3.4 4.1 5.2 0.84 Example 2 4.8 6.2 7.9 1.32 Example 3 2.9 3.6 4.4 0.65 Example 4 3.7 4.9 6.1 1.05 Comparative Example 1 18.5 67.3 142.6 28.74 Comparative Example 2 11.2 45.8 89.4 16.51 Comparative Example 4 86.4 194.2 315.8 54.27

[0149] Figure 4 This is a test chart of the extreme high hardness water quality tolerance and phase stability of the present invention, which includes two sub-charts. Sub-chart (a) shows the trajectory of the macroscopic turbidity change of the liquid phase of each group of samples after adding 1000 mg / L artificial hard water and standing for 0 to 72 hours. The densely distributed solid line group below represents Examples 1 to 4, and the discrete and steeply sloped dashed line group above represents the three comparative examples; Sub-chart (b) visually maps the mass percentage of solid precipitate stripped from each system under centrifugal force field after the standing period through a needle-like discrete plot.

[0150] According to the data in Table 4, high-hardness groundwater is highly susceptible to becoming a destructive factor that disrupts the phase equilibrium of the pesticide system in livestock end-use scenarios. In routine disinfection operations at farms, pesticide solutions often need to be prepared in advance in a mixing tank and allowed to stand before spraying. This time window presents a severe test to the salt-out resistance of the formulation. The samples in Examples 1 to 4, after being immersed in extreme metal ions for up to 72 hours, consistently maintained turbidity at extremely low single-digit levels, and the proportion of precipitate extracted by centrifugation did not exceed the critical threshold of 1.5%. This excellent environmental tolerance stems directly from the pre-constructed multidentate sacrificial coordination network within the system. The densely packed free phenolic hydroxyl and carboxyl groups on the macromolecular backbone of sodium lignosulfonate constitute a massive three-dimensional chelating trap, preferentially depriving free calcium and magnesium ions from penetrating the aqueous phase. This forces these highly cross-linked polyvalent metal ions to be bound to the polymer periphery, preventing them from penetrating to the core region to disrupt the already stably assembled "alkaloid-adjuvant" ion-pair complex.

[0151] Test Example 5: Determination of the aqueous retention rate of the active ingredient (matrine)

[0152] This test case mainly focuses on Example 1 and Comparative Example 5, tracking the redistribution of core bactericidal active molecules between the liquid phase and the precipitate phase after extreme water aging and settling, thereby verifying the key role of acidification protonation pretreatment in preventing the effective components from being "swept and co-precipitated".

[0153] 1. Collect the suspensions of Example 1 and Comparative Example 5 after standing for seventy-two hours in Test Example 4. Without disturbing the bottom sediment, extract the supernatant sample and push it through a polytetrafluoroethylene microporous filter membrane with a pore size of 0.45 micrometers to retain any micron-sized flocs that may remain in the liquid phase.

[0154] 2. Transfer the purified filtrate to a standard chromatographic vial and place it in the autosampler tray of a high-performance liquid chromatograph equipped with a UV detector for analysis.

[0155] 3. Set the chromatograph operating parameters, using a C18 reversed-phase column as the stationary phase, and the mobile phase is prepared as an isocratic elution system of methanol and phosphate buffer containing 0.1% triethylamine. The column temperature is kept constant at 30 degrees Celsius, the flow rate is set to 1.0 mL per minute, and the detection wavelength is locked at 208 nm.

[0156] 4. Pre-inject high-purity matrine standard solutions of varying concentrations, and establish a linear working curve based on retention time and chromatographic peak area fitting.

[0157] 5. Perform five independent parallel injections on each group of samples, record the corresponding characteristic peak areas and substitute them into the standard curve equation, calculate the actual free matrine concentration in the aqueous phase in reverse, and finally divide by the theoretical initial concentration calculated based on the feed amount to output the relative retention rate matrix of effective components.

[0158] Table 5 Independent parallel test data on matrine retention rate in aqueous phase after 72 hours of aging in extreme hard water.

[0159] Parallel determination 1 418.5 93.8 176.2 39.5 Parallel determination 2 424.3 95.1 187.8 42.1 Parallel determination 3 413.6 92.7 170.4 38.2 Parallel determination 4 422.1 94.6 194.5 43.6 Parallel measurements 5 429.2 96.2 181.9 40.8

[0160] Figure 5 This is a distribution chart of the retention rate of effective components after extreme water aging of the present invention. The dark circular scatter dots on the left side of the chart represent the distribution of matrine retention rate in five parallel determinations of Example 1, and the light square scatter dots on the right side represent the distribution of Comparative Example 5. The thick black horizontal line corresponds to the mathematical expectation mean of the two groups of samples, and the extended vertical line segment represents the standard deviation of data fluctuation.

[0161] According to the data in Table 5, the changes in turbidity in the macroscopic phase are ultimately directly mapped onto the spatial distribution of the core active substances in the microscopic dimension. In the actual disinfection operation environment of the farm, the final killing efficacy of the disinfectant does not depend on the theoretical amount of material added on the original formula of the factory, but is highly dependent on the concentration of free molecules actually dissolved in the aqueous medium and successfully reaching the target surface with the micro-mist droplets. In Example 1, after experiencing extreme hard water chemical stress for up to 72 hours, the concentration signal of matrine captured by the high performance liquid chromatograph in multiple parallel samplings remained at an extremely high baseline, with an average relative retention rate exceeding 94%. This excellent anti-precipitation ability can be traced back to the artificially created acidic time window at the front end of the preparation process. A large number of free hydrogen ions forcibly occupy the hydrogen bond acceptor sites on the original tannin molecular structure in the plant extract, forcing matrine to dissociate and recombine into quaternary ammonium salt free ions with a net positive charge. The subsequently introduced sodium lignosulfonate, relying on the high density of sulfonic acid groups on its molecular backbone, irreversibly captures and anchors these protonated alkaloids with electrostatic attraction far exceeding that of natural hydrogen bonds, firmly embedding them within the three-dimensional hydration network of the anionic polymer. Even if an overload of polyvalent metal ions in the water body causes salting-out of free impurities or some residual polyphenols, the core alkaloids, having completed their charge binding, can avoid the risk of phase transfer and maintain a good aqueous solubility.

[0162] Test Example 6: Simulation Test of Attenuation Rate During Continuous Operation of Automated Micro-Mist Nozzle

[0163] This test case mainly focuses on the diluted solutions of Example 1, Comparative Examples 6 and 7. Using a high-pressure fluid test platform built to simulate a farm environment, it evaluates the mechanical permeability of fluids with subtle mesoscopic structural differences when encountering extreme spatial compression and strong shear flow fields, so as to reflect the risk of blockage in real industrial pipelines.

[0164] 1. Take the final preparations of Example 1, Comparative Example 6 and Comparative Example 7 respectively, and inject them into simulated groundwater containing high concentrations of free calcium and magnesium ions according to the 1:300 ratio commonly used in livestock farms. Turn on the impeller agitator to mix them thoroughly to prepare the working mother liquor to be tested.

[0165] 2. After homogenization, each group of mother liquor is pumped into three completely independent stainless steel storage tanks with constant temperature jackets. The entire liquid supply system is then connected to a high-pressure spray circuit pre-configured with an industrial-grade ceramic plunger pump.

[0166] 3. Adjust the bypass valves of each circuit to force the working pressure in the pipeline system to be kept constant at the industrial standard value of 5.0 MPa, and connect a 304 stainless steel micro-mist nozzle with a nominal orifice diameter of 50 micrometers to the fluid end, and then start the system to enter the closed continuous circulation spraying state.

[0167] 4. Using a high-frequency electromagnetic flowmeter attached to the nozzle inlet section, the real-time fluid throughput is captured and the average value is calculated at five consecutive minutes at the initial zero moment of equipment operation and at the 12th, 24th, 48th and 72nd hour nodes thereafter.

[0168] 5. Based on the absolute values ​​of the flow rate at each time section, calculate the percentage decrease in volumetric flow rate relative to time zero, thereby quantifying the hydrodynamic blockage effect of the internal microscopic suspended structure in a micrometer-level confined space.

[0169] Table 6. Test data of absolute flow rate and attenuation rate during continuous operation of the micro-mist nozzle.

[0170] Example 1 124.6 124.2 123.5 123.8 122.9 1.36 Comparative Example 6 125.1 118.4 106.2 93.5 87.1 30.38 Comparative Example 7 124.8 102.3 74.6 58.2 41.5 66.75

[0171] Figure 6 This is a simulation test chart of the continuous operation attenuation rate of the automated micro-mist nozzle of the present invention, consisting of two vertically arranged sub-charts. Sub-chart (a) records the time series evolution of the absolute flow rate in the microporous channel driven by the high-pressure pump. The solid line corresponds to the extremely gentle trajectory of Example 1, while the dashed line and dotted line respectively delineate the flow rate decline process of Comparative Example 6 and Comparative Example 7 when encountering gradual blockage. Sub-chart (b) visually displays the percentage of accumulated resistance attenuation in each system pipeline after three days of continuous operation through discrete needle-shaped markers.

[0172] According to the data in Table 6, the apparent clarity of a fluid under macroscopic static conditions is not directly equivalent to its engineering reliability under extreme hydraulic conditions. In the highly automated disinfection process of modern animal husbandry, high-pressure plunger pumps force the liquid medicine through extremely fine nozzle orifices. This constricted flow channel places extremely high demands on the mesoscopic homogeneity of the liquid. After three days of high-load cycling, the test pipeline in Example 1 maintained an almost flat baseline at the terminal flow rate, and the final system attenuation rate was firmly suppressed to within 1.4%. This excellent hydrodynamic penetration performance directly reflects the theoretical effectiveness of the slow acid adjustment combined with high shear intervention in the previous process. Because the gel network inside the system is completely torn apart by the rapidly rotating dispersion disc, and the slow pH adjustment gives the surfactant sufficient adsorption and encapsulation time, the generated effective drug-loaded particles are not only extremely small in size, but their dense nano-hydration layer provides excellent resistance to deformation and slippage, ensuring that the fluid can smoothly slide through the 50-micron physical pores without mechanical retention.

[0173] Test Example 7: Evaluation of the quantitative bactericidal efficacy of suspension under extreme high hardness water quality interference

[0174] This test case mainly focuses on the final formulations of Example 1, Comparative Examples 4 and 5. Based on the environmental stress simulation of a specific water quality aging cycle, it quantitatively examines the ability of the formulations to maintain their macroscopic biological killing efficacy when facing the harsh groundwater dilution scenario of a real aquaculture farm, in order to verify the direct mapping relationship between microscopic physical phase stability and final antimicrobial function in a closed loop.

[0175] 1. Standard test strains of *Escherichia coli* (ATCC25922), *Salmonella* (ATCC14028), *Staphylococcus aureus* (ATCC6538), and *Streptococcus* (ATCC19615) in the logarithmic growth phase were selected. The bacterial suspensions were repeatedly centrifuged, eluted, and resuspended in sterile physiological saline containing 0.1% Tween-80. The baseline concentration of the bacterial suspensions was precisely adjusted to 1.5 × 10⁻⁶ using the McFarland turbidimetric method combined with a spectrophotometer. 8 Up to 3.0×10 8 Within the specified range of CFU / mL.

[0176] 2. Take 4.5 ml of the test drug solution samples from Examples 1, Comparative Example 4 and Comparative Example 5, which were diluted with 1000 mg / L extremely hard artificial groundwater at a volume ratio of 1:300 and subjected to 0 hours and 72 hours of dark static aging respectively. Transfer them into sterile stoppered test tubes and place them in a constant temperature biochemical water bath at 20 degrees Celsius for preheating and equilibration.

[0177] 3. Quickly inject 0.5 ml of the aforementioned standardized target bacterial suspension into each test tube, mix at a moderate speed using a micro vortex mixer for five seconds, and immediately start a stopwatch to precisely time the mixture, maintaining a strict ten-minute physical contact time between the drug and the microbial target in the liquid environment.

[0178] 4. After reaching the set 10-minute contact point, quickly aspirate 0.5 ml of the reaction solution using a micropipette and inject it directly into a specific neutralizing broth containing 4.5 ml of a compound of polysorbate 80, lecithin, and sodium thiosulfate (ratio: polysorbate 80: 3.0%; lecithin: 0.3%; sodium thiosulfate: 0.5%). Thoroughly vortex the mixture to completely stop any remaining drug molecules from penetrating and disrupting the cell walls.

[0179] 5. The neutralized bacterial solution was serially diluted tenfold with sterile physiological saline. Three appropriate dilution gradients were selected, and 100 μL of each gradient was spread onto tryptone soybean agar plates. After the liquid had completely penetrated the culture medium, the plates were inverted and incubated in a 37°C incubator for 48 hours.

[0180] 6. After the culture period ended, extract the agar plates, use an automatic colony counter to screen out diffuse and small background interference points, count the total number of effective surviving colonies that meet the technical specifications in each group and perform logarithmic transformation. Combine the initial viable bacteria data using hard water as a negative control group, calculate the true log killing value of each drug system at different aging time points.

[0181] Table 7. Measured quantitative logarithmic killing values ​​of target strains in each system before and after aging in extreme hard water.

[0182] Example 1 E. coli 5.82 5.61 Comparative Example 4 E. coli 4.15 1.28 Comparative Example 5 E. coli 5.43 2.14 Example 1 salmonella 5.75 5.58 Comparative Example 4 salmonella 4.08 1.22 Comparative Example 5 salmonella 5.36 2.05 Example 1 Staphylococcus aureus 6.14 5.87 Comparative Example 4 Staphylococcus aureus 4.31 1.45 Comparative Example 5 Staphylococcus aureus 5.65 2.42 Example 1 Streptococcus 6.05 5.82 Comparative Example 4 Streptococcus 4.25 1.38 Comparative Example 5 Streptococcus 5.58 2.35

[0183] Figure 7 This is a dumbbell diagram showing the decline in the bactericidal efficacy of each system against the target bacterial strains after aging in extremely hard water according to the present invention. The diagram uses horizontal dashed lines to integrate the test data for Escherichia coli, Salmonella, Staphylococcus aureus, and Streptococcus into a vertical distribution on the same coordinate system. Hollow circles represent the initial bactericidal efficacy of each drug system immediately after dilution in extremely hard water, while solid circles reveal the final efficacy retention level after 72 hours of static aging. The thick black solid line connecting two points visually maps the range of efficacy decline induced by water quality stress.

[0184] Based on the quantitative microbial killing data shown in Table 7, the differences in the microscopic phase structure exhibited by the drug system in the preliminary validation are ultimately directly reflected in the macroscopic biological killing efficacy. Conventional laboratory efficacy testing defaults to using deionized water or low-hardness standard water as the dilution medium. This operating condition cannot truly reflect the efficacy attenuation problem that occurs when natural plant extract compound is exposed to the high-hardness water environment of aquaculture farms. After being immersed in a 1000 mg / L high-calcium-magnesium ion system for 72 hours, the sample from Example 1 maintained an effective level of over 5.5 in killing Gram-negative Escherichia coli and Salmonella, or Gram-positive Staphylococcus aureus and Streptococcus. The mechanism maintaining this antimicrobial activity lies in the pre-protonation induction combined with macromolecular network assembly, ensuring that the free core alkaloids are not dislocated or stripped due to the intervention of metal ions. The active ingredient, which is electrostatically anchored to the periphery of the microparticle, retains spatial freedom. When the drug-loaded microparticle comes into contact with the bacterial cell membrane with the fluid, the positively charged quaternary ammonium salt groups can attach to and destroy the negatively charged phospholipid bilayer, thus killing the pathogen within a ten-minute contact period.

[0185] Comparative Example 4, which did not undergo native substrate deconstruction, showed a bactericidal logarithmic value only slightly above 4.0 at instantaneous mixing with hard water, indicating a retention effect of the natural hydrogen bond network in the plant extract on the release of active ingredients. Alkaloids not released by strong acid were nested within clusters of large-molecule polyphenols, preventing the release of lethal doses of active substances into the liquid phase. Comparative Example 5, lacking acidification and network recombination processes, exhibited efficacy loss due to uncontrolled microscopic phase transitions. This group showed some bactericidal performance in its initial diluted state, but as the hard water aging period lengthened, polyvalent metal ions triggered flocculation and precipitation of polyphenol components, leading to co-precipitation of effective bactericidal molecules in the aqueous phase. This physical phase transition resulted in a significant decrease in the bactericidal logarithmic value after 72 hours, dropping to the 2.0-2.4 range. This phenomenon explains the loss of efficacy of some compound disinfectant products in on-site static storage tanks. Comparison of test data shows that molecular-level deconstruction and secondary assembly of plant substrates during the preparation stage is a necessary technical approach for establishing a long-lasting bactericidal barrier in harsh water quality environments.

[0186] 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 compound disinfectant made from traditional Chinese medicine for disinfecting the environment of livestock and poultry farms, characterized in that, It contains the following components by mass percentage: Deionized water 35-67%; 10-20% total alkali water extract of Sophora flavescens; Artemisia argyi aqueous extract concentrate 10-20%; Sodium lignosulfonate 3-8%; Alkyl polysaccharide 5-10%; Citric acid aqueous solution 1-4%; 2-5% sodium citrate aqueous solution; The disinfectant is prepared by the following steps: first, the pH of the system is adjusted to 3.8-4.2 to induce the protonation of alkaloids, then sodium lignosulfonate is added to anchor the active ingredients through electrostatic interaction, followed by the addition of alkyl polysaccharides to form a hydration coating layer, and finally the pH is gradually increased to 5.5-6.0 to solidify the structure.

2. The herbal compound disinfectant for disinfecting livestock and poultry farm environments according to claim 1, characterized in that, The preferred mass percentage ratio of the components is any one of the following: Formula 1: 52% deionized water, 15% concentrated total alkali extract of Sophora flavescens, 15% concentrated water extract of Artemisia argyi, 5% sodium lignosulfonate, and 8% alkyl polysaccharide glycosides; Formula 2: 67% deionized water, 10% concentrated total alkali extract of Sophora flavescens, 10% concentrated water extract of Artemisia argyi, 3% sodium lignosulfonate, and 5% alkyl polysaccharide glycosides; Formula 3: 35% deionized water, 20% concentrated total alkali extract of Sophora flavescens, 20% concentrated water extract of Artemisia argyi, 8% sodium lignosulfonate, and 10% alkyl polysaccharide glycosides.

3. The herbal compound disinfectant for disinfecting livestock and poultry farm environments according to claim 1, characterized in that, The solid content of the total alkaloid aqueous extract of Sophora flavescens and the aqueous extract of Artemisia argyi are both limited to 20%; and the mass concentration of the citric acid aqueous solution and the sodium citrate aqueous solution are both 20%.

4. The herbal compound disinfectant for disinfecting livestock and poultry farm environments according to claim 3, characterized in that, The total alkali water extract concentrate of Sophora flavescens is obtained by a specific extraction process including the following steps: adding ten times the amount of deionized water and boiling gently for two hours to filter out the first extract; adding eight times the amount of deionized water to the residue and boiling gently for one and a half hours to filter out the second extract; combining the two extracts and then concentrating under reduced pressure at 60°C and a vacuum of -0.08MPa to obtain the final extract.

5. A method for preparing a compound disinfectant solution of traditional Chinese medicine for disinfecting the environment of livestock and poultry farms according to any one of claims 1, characterized in that, Includes the following sequential steps: S1 Initial Dispersion and Forced Protonation: Deionized water, concentrated total alkaloids of Sophora flavescens and concentrated water extract of Artemisia argyi were mixed in a mixing tank, and low-speed stirring was started. Citric acid aqueous solution was added dropwise to lower the pH value of the system to squeeze out hydrogen bond acceptor sites and induce protonation and recombination of alkaloids. S2 Heating Depolymerization and Polymer Anchoring: The reaction system is heated and kept at a constant temperature, and a pre-dissolved sodium lignosulfonate solution is continuously added dropwise. During this process, the high-speed dispersion disk in the inner ring is triggered by the sudden change feedback of the current baseline of the low-speed stirring motor to carry out network depolymerization under a high shear flow field, and the endpoint of colloidal depolymerization is determined based on online conductivity data. S3 Cooling and Homogenization and Hydration Layer Construction: The temperature inside the reactor is lowered, alkyl polysaccharide is added and stirred and homogenized while maintaining a moderate shear rate; S4 Closed-Loop Constant-Rate Alkali Adjustment: An online pH meter and metering pump are linked in a closed loop to limit the rate of pH increase. Sodium citrate solution is added dropwise to allow the system to solidify its structure in a gentle pH gradient. S5 maturation and fine filtration: After continuous low-speed stirring and maturation, the product is filtered and filled to obtain the finished product.

6. The method for preparing a compound disinfectant solution of traditional Chinese medicine for disinfecting the environment of livestock and poultry farms according to claim 5, characterized in that, In step S1, the temperature of the system material is controlled at 20-30℃, and the apparent shear rate is set to 100-150s. -1 Furthermore, the pH value of the system is adjusted and stabilized between 3.8 and 4.2 by adding citric acid aqueous solution dropwise, and the effect is maintained for 20-30 minutes.

7. The method for preparing a compound disinfectant solution of traditional Chinese medicine for disinfecting the environment of livestock and poultry farms according to claim 5, characterized in that, The specific implementation method of the depolymerization process in step S2 is as follows: the material is heated to 60-70℃; sodium lignosulfonate is pre-dissolved in deionized water and added dropwise at a constant rate over 20-30 minutes; the current of the low-speed stirring motor is monitored in real time, and when the current value increases by more than 30% compared with the baseline before addition, the high-speed dispersion disk with a shear rate of 600-800s⁻¹ is triggered to run for 3-5 minutes, and automatically shut off when the current drops back to within ±5% of the baseline; the online conductivity data after temperature compensation is continuously recorded, and the heating source is cut off when the relative decrease rate of conductivity is less than 2.0% within 10-15 minutes.

8. The method for preparing a compound disinfectant solution of traditional Chinese medicine for disinfecting the environment of livestock and poultry farms according to claim 5, characterized in that, In step S3, the cooling target is set at 30-40°C, and the alkyl polysaccharide is applied for 150-200 seconds. -1 Stir and homogenize at a shear rate for 15-20 minutes; in step S4, the pH increase rate is controlled at 0.1-0.2 pH units / minute, and the addition of sodium citrate solution is stopped when the pH value of the system slowly rises and stabilizes at the target threshold of 5.5-6.

0.

9. The method of using a compound disinfectant solution of traditional Chinese medicine for disinfecting the environment of livestock and poultry farms according to any one of claims 1, characterized in that, Includes the following steps: The herbal compound disinfectant solution was mixed with the groundwater medium in the breeding area at a volume ratio of 1:300 to prepare a diluted working stock solution. The diluted working mother liquor is pumped into a high-pressure spray circuit equipped with a plunger pump, forcibly maintaining the working pressure in the pipeline system at 5.0 MPa. The end is applied to the aquaculture environment through a micro-mist nozzle with a nominal orifice diameter of 50 μm to avoid the shear condensation effect in the confined flow channel and maintain continuous flow.

10. The method of using a compound disinfectant solution of traditional Chinese medicine for disinfecting the environment of livestock and poultry farms according to claim 9, characterized in that, The groundwater medium in the breeding area is extremely hard water that is attacked by polyvalent metal ions and has a total hardness of no more than 1000 mg / L (calculated as calcium carbonate); the diluted working mother liquor, after standing in the above-mentioned hard water medium for 72 hours, has a liquid phase turbidity of no more than 7.9 NTU and a mass retention rate of matrine in the aqueous phase of more than 90%.