Method for preparing ultra-high-purity nanoscale total bamboo leaf flavonoid dispersion

Abstract

The present invention belongs to the technical field of the extraction of total bamboo leaf flavonoids, and relates to a method for preparing an ultra-high-purity nanoscale total bamboo leaf flavonoid dispersion. The method comprises the following steps: (1) extracting a nanoscale bamboo leaf flavonoid compound by using an integrated device for superfreezing-assisted high pressure-double vortex countercurrent back-pressure cavitation continuous dynamic cyclic nano-grinding and wall-breaking extraction and filtration; (2) subjecting same to adsorption separation and dynamic elution and desorption by means of a combination of ionic liquid functionalized vortex magnetic nano-elliptic hollow ring balls and an external rotating magnetic field; (3) performing low-temperature vacuum evaporation and concentration; and (4) freeze-drying same to prepare an ultra-high-purity nanoscale total bamboo leaf flavonoid dispersion with D50 of 0.02-0.08 μm and a purity of 99.7-99.9%. The method has overcome the limitations of an industrial technique for extracting flavonoids from bamboo leaves, achieves large-scale industrialization of an ultra-high-purity nanoscale total bamboo leaf flavonoid dispersion, and is used in the fields of active pharmaceutical ingredients, health products, food products for special needs, drink products with special functions, cosmetics, etc.

Description

A method for preparing ultra-high purity nano-scale bamboo leaf total flavonoids dispersion Technical Field

[0001] The invention relates to a method for preparing an ultra-high-purity nano-scale bamboo leaf total flavonoids dispersion, in particular to a method for preparing an ultra-high-purity nano-scale bamboo leaf total flavonoids dispersion, and belongs to the technical field of bamboo leaf total flavonoids extraction. Background Art

[0002] According to patents and public documents in this field, the current status of bamboo leaf flavonoid extraction technology research at home and abroad is as follows:

[0003] A method for preparing bamboo leaf flavonoids extract by column purification (200910223926.6) shows that the purity of bamboo leaf flavonoids is 20.78%; a production method for extracting bamboo leaf flavonoids from bamboo leaves (200610053134.5) shows that the purity of bamboo leaf flavonoids is ≥24%; a method for separating and purifying flavonoids and lactones from bamboo leaves based on microwave-assisted technology (CN201510481490) shows that the purity of bamboo leaf flavonoids is ≥29%; a method for preparing bamboo leaf flavonoids extract (200910223927.0) shows that bamboo leaf flavonoids The purity is 42%; A method for extracting flavonoids from bamboo leaves 201110003352.9; showing that the purity of bamboo leaf flavonoids is 30-50%; A method for extracting bamboo leaf flavonoids 201110406495.4 showing that the purity of bamboo leaf flavonoids is 30-50%; Production process for extracting bamboo leaf flavonoid series products from bamboo leaves 200610053436.2 showing that the purity of bamboo leaf flavonoids is 60%; Preparation method of bamboo leaf flavonoid extract 200810195064.6 showing that the purity of bamboo leaf flavonoids is 40%-65%;

[0004] Taiyuan University of Technology - Research Progress on Flavonoids in Bamboo Leaves shows that bamboo leaf flavonoid powder with a flavonoid content of 24% was obtained; Central South University of Forestry and Technology - Research on Extraction, Purification and Antioxidant Activity of Bamboo Leaf Flavonoids - The total flavonoid content in the obtained product is 36%; Yangzhou University School of Food Science and Engineering - Research on Physiological Activity and Application of Bamboo Leaf Flavonoids - The obtained bamboo leaf flavonoid content reached more than 40%; Beijing Forestry University School of Biological Sciences and Technology Food Department - Research on Optimization and Analytical Characteristics of Adsorbents in Bamboo Leaf Flavonoid Purification - The purity of bamboo leaf flavonoids produced by this process reached 54.16%; Nanchang University - Pilot Extraction of Active Polysaccharides and Flavonoids from Moso Bamboo Leaves - The purity of moso bamboo leaf flavonoids after refining with AB-8 resin reached 79.4%.

[0005] Therefore, according to conventional technical knowledge in this field and industry consensus, the bamboo leaf flavonoids described above are only a conceptual summary. In fact, it is just a crude extract with a low extraction rate and a large number of impurities during extraction (such as phenols, saponins, tannins, alkaloids, polysaccharides, proteins, crude fat, chlorophyll, anthraquinone compounds, terpenoid lactones, inorganic salts, water, minerals, ash, heavy metals, arsenic and trace elements such as manganese, zinc, selenium, more than 20 mineral elements, 82 aromatic compounds, 16 amino acids, 53 volatile components, 10 alcohols, 17 aldehydes, etc.). The so-called bamboo leaf flavonoids are only a part of the content of these substances and are at best just a trade name.

[0006] Based on the common knowledge in the industry, bamboo leaf flavonoids of different purities have different effects in different fields. The higher the purity of bamboo leaf flavonoids, the stronger their activity and the greater their polarity. To achieve the effects of effectively lowering blood lipids, preventing cardiovascular diseases, improving hypoxia tolerance and preventing osteoporosis, the purity must be at least 90%. Therefore, purity determines the physiological activity of a drug. Therefore, how to prepare high-purity flavonoids at low cost is currently the focus of research by scientists from all over the world. Therefore, how to extract them from natural materials efficiently, economically and environmentally friendly is a problem that should be solved in the production of large quantities of high-quality flavonoids.

[0007] In summary, although there have been certain achievements in the extraction of bamboo leaf flavonoids, the purity of the flavonoid products of existing manufacturers is relatively low, and it brings a lot of trouble to further separation. The subsequent refining process is relatively cumbersome and time-consuming. The market can only use this purity for the health care of anti-fatigue and improving human function, thus limiting its further development in the food and pharmaceutical fields. There are also certain limitations in industrial application. How to quickly and efficiently industrialize and scale up the production of bamboo leaf flavonoids is the focus of our research. Summary of the Invention

[0008] Therefore, in actual production, finding a new process for extracting effective components from bamboo leaves with high purity, high efficiency, low cost and low pollution has become a problem of concern. In order to overcome the limitations caused by the shortcomings of existing technologies at home and abroad, this application focuses on developing a new method. This application designs a method for preparing an ultra-high purity nano-scale bamboo leaf total flavonoid dispersion:

[0009] ① Carry out a thorough reform of extraction equipment and auxiliary materials to reasonably and effectively improve product extraction rate, reduce production costs, and facilitate industrial production;

[0010] ② The orthogonal test analysis method was used to optimize the process conditions for extracting total flavonoids from bamboo leaves in this application. According to the characteristics of each extraction technology, integrated research between different extraction technologies or between extraction technology and separation technology was carried out to diversify the development of extraction technology and better provide technical support for screening the best process;

[0011] The nanoparticle size median D 50 =0.02-0.08 μm, and the extraction technology of nano-scale ultra-high purity bamboo leaf total flavonoids dispersion with a purity of 99.7-99.9% has not been reported before, and is the first case before this application; it provides a theoretical reference for better development and utilization of my country's abundant bamboo leaf resources.

[0012] In order to achieve the above-mentioned purpose, the technical solution adopted in this application includes the following process steps:

[0013] Step 1: Ultra-low temperature freezing assisted high pressure-double vortex countercurrent back pressure cavitation continuous dynamic circulation nano-grinding wall breaking extraction and filtration integrated device to extract nano-scale bamboo leaf flavonoids:

[0014] The refrigerant is input into the jacket layer of the integrated device, the cascade ultra-low temperature freezing system is started, and the cooling temperature in the pear-shaped grinding and wall-breaking extraction tank is adjusted to -15°C to -50°C; bamboo leaf powder, 30-90% ethanol solution, 4-5 parts of bioflocculant solution, and grinding media with a filling rate of 70-80vol% are placed into the pear-shaped grinding and wall-breaking extraction tank at a material-liquid ratio of 1:10-20g / mL, and the double-turbine forward and reverse vortex countercurrent drive disk is turned on and rotated at a high speed of 12-20m / s. At the same time, the pressure pump is turned on to press the inert gas into the pear-shaped grinding and wall-breaking extraction tank, and the pressure is adjusted to 0.5-2.5MPa. The air flow rate is 200L / min, and the whole process participates in the ultra-low temperature continuous dynamic circulation. The total time for the ring grinding and wall breaking / extraction treatment is 30 to 50 minutes. At the 15th minute of the total treatment time, the peristaltic pump is started, and a 30-90% ethanol solution with a material-liquid ratio of 1:10-20 g / mL is continuously and dynamically added dropwise within 10 to 30 minutes, ultimately reaching a total processing volume of 1:20-40 g / mL material-liquid ratio. The pressure is then released, and the material is discharged from the discharge port of the pear-shaped grinding and wall breaking extraction tank to the solid-liquid separation nanofiltration layer, which is subjected to high-speed rotation and intermittent compression motion. Under the action of centrifugal force, the filtrate passes through the nanofiltration rotary membrane in a tangential manner under the pressure of the pump and 3 to 5 kg, and flows out from the bottom of the integrated device through the hollow pipe, achieving solid-liquid separation. The median particle size D 50 = 0.02-0.08 μm nanoscale bamboo leaf flavonoid solution and solid bamboo powder precipitate;

[0015] The refrigerant is any one of 30-80% ethanol and liquid nitrogen;

[0016] The grinding medium is a zirconia ball or a ceramic ball, and the diameter of the grinding medium ranges from 0.2 to 0.4 mm;

[0017] The bioflocculant solution is any one of 1% gelatin solution and 1% chitosan solution;

[0018] The inert gas is any one of carbon dioxide, argon, and food grade 99.999% ultrapure nitrogen;

[0019] The nanofiltration rotary membrane is a microporous filter membrane with a pore size of 0.02 to 0.08 μm;

[0020] Step 2: Ionic liquid functionalized vortex magnetic nano-elliptical hollow ring combined with an external rotating magnetic field for adsorption separation and dynamic elution and desorption:

[0021] The nanoscale bamboo leaf flavonoid compound solution of step 1 and the ionic liquid functionalized vortex magnetic nano-elliptical hollow ball are evenly mixed in a ratio of 5:1, filled in a polytetrafluoroethylene tube, ultrasonicated at 30°C for 5 minutes, and flowed through the resin column at a flow rate of 3BV / h until adsorption saturation. An annular cylindrical external rotating magnetic field is applied close to the tube wall, and the magnetic induction intensity of the external rotating magnetic field is 1 to 1.5T. After vortexing for 20 minutes, the external rotating magnetic field is turned off; 5BV of distilled water and 5BV of 30% ethanol are used to elute the impurities of the flavonoid adsorbent on the resin column, respectively, and then the flavonoids are further eluted with 5BV of 50% ethanol and 4BV of 70% ethanol, respectively, to finally achieve complete desorption, and the total elution and desorption time is 25 minutes; the 50% and 70% ethanol eluates are combined, and then filtered and the desorbed liquid is collected;

[0022] The ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere is any one of Fe3O4@HDI-EMIMLpro and Fe3O4@SiO2@HDI-EMIMLpro;

[0023] The ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere is prepared by:

[0024] ⑴In a sealed reactor, Fe 3+ As a reactant, phosphate and sulfate surfactants are introduced. Under high temperature and high pressure conditions, supersaturation and crystal precipitation occur. PO4 3- and SO4 2-They selectively adsorbed on the crystal faces of α-Fe2O3 crystals, inducing the iron oxide crystals to form a polyhedral structure and preferentially dissolving it along the long axis to form a hollow structure. By adjusting the concentration of the reactants and the auxiliary magnetic field, the nanowires were oriented and arranged, prompting the composite particles to form nano-elliptical hollow balls with an aspect ratio β = 1.5. Furthermore, using the α-Fe2O3 nano-elliptical hollow balls as precursors, Fe3O4 vortex magnetic nano-elliptical hollow balls with good dispersion, high phase purity and magnetic anisotropy were obtained through hydrogen thermal reduction method.

[0025] (2) Using tetraethyl orthosilicate as a precursor solvent to coat a thin layer of silicon dioxide SiO2 on its surface, thereby obtaining a Fe3O4@SiO2 composite vortex magnetic nano-elliptical hollow sphere with good dispersion;

[0026] ⑶ Using hexamethylene diisocyanate (HDI) as a linker, the amino acid ionic liquid 1-ethyl-3-methylimidazole L-proline salt (EMIMLpro) was modified on the surface of Fe3O4 vortex magnetic nano-ellipsoidal hollow rings and Fe3O4@SiO2 composite vortex magnetic nano-ellipsoidal hollow rings, respectively, to obtain two ionic liquid-functionalized vortex magnetic nano-ellipsoidal hollow rings, Fe3O4@HDI-EMIMLpro and Fe3O4@SiO2@HDI-EMIMLpro; the nano-ellipsoidal hollow ring with an aspect ratio β = 1.5 has an outer major axis a = 90-100 nm, an outer minor axis b = 60-66 nm, an inner major axis a = 72-80 nm, an inner minor axis b = 48-53 nm, and an inner and outer diameter thickness of 9-10 nm;

[0027] Step 3: Low temperature vacuum evaporation and concentration:

[0028] The desorption liquid from step 2 is fed into a low-temperature vacuum evaporation and concentration device to remove water and ethanol from the desorption liquid to obtain a concentrate;

[0029] Step 4: Freeze-drying:

[0030] The concentrate obtained in step 3 was freeze-dried to obtain a particle size D 50 = 0.02-0.08 μm, nano-scale ultra-high purity bamboo leaf total flavonoids dispersion with a purity of 99.7-99.9%;

[0031] The method for detecting the median particle size is to use a laser particle size analyzer to perform wet particle size detection in accordance with GB / TT19007:2016, ISO 13320:2009, and Q / 0100JWN001-2018;

[0032] The purity is detected by high performance liquid chromatography (HPLC) according to the high performance liquid chromatography method (General Rule 0512 of the 2020 edition of the Chinese Pharmacopoeia).

[0033] The ultra-low temperature freezing-assisted high pressure-dual vortex countercurrent back pressure cavitation continuous dynamic cycle nano-grinding wall breaking extraction and filtration integrated device described in step 1 is composed of a pear-shaped grinding wall breaking extraction tank, a jacket layer and a solid-liquid separation nanofiltration layer;

[0034] The pear-shaped grinding and wall-breaking extraction tank adopts a double-turbine forward and reverse vortex countercurrent drive motion mode, with an inner radius of 60mm, a depth of 938mm, and a specific surface area of ​​0.01;

[0035] The jacket layer is provided with input and output sealing covers, and the input sealing cover is equipped with an electromagnetic valve. The refrigerant is directly introduced into the jacket layer through the pump body to directly cool it. After the refrigerant absorbs heat, it is discharged through the electromagnetic valve installed on the output sealing cover, so that the pear-shaped grinding and wall-breaking extraction tank filled with materials is in a certain constant temperature and low temperature environment; the temperature is externally controlled, with a temperature control accuracy of ±0.5°C and a temperature control range of 4 to -100°C;

[0036] The solid-liquid separation nanofiltration layer is a special structure of high-speed rotation and intermittent compression motion filtration.

[0037] The freeze drying in step 4 is any one of vacuum freeze drying and spray freeze drying.

[0038] The nano-scale ultra-high purity bamboo leaf total flavonoids dispersion has a median particle size of D 50 =0.02~0.08μm, purity is 99.7~99.9%, and it is used in medicine, health care products, special food, special function beverage, and cosmetics as needed.

[0039] The solid bamboo powder precipitate described in step 1 is powdered by pressure spray drying or cyclone combined pressure spray drying, and is applied in the fields of composite materials, bioplastics, motor vehicle shells and interiors, coatings and inks, water purification, bioethanol, petrochemicals, tobacco, explosives, and nanocellulose products. Beneficial effects

[0040] This application pioneered the use of ultra-low temperature freezing assisted high pressure-double vortex countercurrent back pressure cavitation continuous dynamic circulation nano-grinding wall breaking extraction and filtration integrated device to extract nano-scale bamboo leaf flavonoids.

[0041] From the perspective of plant cell structure, plant cells have a relatively strong cell wall structure; as a protective layer of the cell, the cell wall effectively prevents the release of many intracellular substances; therefore, effective cell wall breaking is a key link in releasing and extracting high-value-added material products contained in the cells; and the key to obtaining useful substances inside the cells is to be able to effectively destroy the cell wall.

[0042] At present, the use of ultrasound to break cell walls is only common in laboratories; however, ultrasonic wall breaking technology requires a large power when processing a large number of cells, and due to the uneven energy distribution of the ultrasonic field, in areas with insufficient energy, the shear force on the cells is small, and the wall breaking effect cannot be achieved, or the wall breaking rate is low; in areas with excessive energy, although a certain wall breaking rate requirement can be achieved, the excessively concentrated energy causes the area to easily heat up too high, which will damage the substances in the cells; the uneven energy distribution of the ultrasonic field leads to a low overall wall breaking rate and greater damage to the useful substances to be extracted; in large-scale industrial production, if ultrasonic wall breaking is used alone, the problems of uneven energy distribution and difficulty in heat dissipation will become more serious, and will also have a greater impact on the product; therefore, it has not yet been applied in industry; to be used in large-scale production, the amplification problem of related engineering equipment needs to be further resolved.

[0043] When using the enzymatic lysis method for cell wall disruption, due to the complex components in the extract, the enzyme may react chemically with certain components in traditional Chinese medicine to produce new chemical substances, thereby affecting the purity and yield of the product; the specificity of the enzyme requires the selection of different enzymes to disrupt different types of cells, resulting in poor versatility of the enzymatic lysis method. In addition, the price of biological enzymes is relatively high, which increases production costs, and the time required for cell wall disruption by the enzymatic lysis method is relatively long. These factors seriously limit the application of the enzymatic lysis method in large-scale industrial processing; therefore, the enzymatic lysis method is generally only suitable for small-scale experimental cell wall disruption and currently does not have the conditions for large-scale industrial production.

[0044] Chemical permeation depends on the structural composition of the cell wall and the type of chemical reagent. Different chemical reagents have different effects on different types of cells, that is, they are selective. Therefore, chemical permeation has poor versatility and also has problems of long processing time and low efficiency. Chemical reagents such as acids, alkalis or oxidants can easily damage the products in the cells. In addition, general chemical reagents have certain toxicity. During the chemical wall breaking process, they can easily contaminate the products, increasing the difficulty of subsequent separation or removal of these reagents. The existence of these problems determines that chemical treatment methods are not suitable for general large-scale industrial production.

[0045] High-pressure homogenization is more suitable for breaking the cell walls of microorganisms. However, the difficulty of breaking is undoubtedly determined by the mechanical strength of the cell wall. For natural plants, the active ingredients are often embedded in internal thin-walled cells or vacuoles protected by hard or soft epidermis. High-pressure homogenization is difficult to destroy the relatively hard cell walls; breaking the cell walls using this method is very difficult.

[0046] The traditional rotor structure bead mill has poor fluidity in the grinding chamber. As the cell wall breaking process continues, the components in the cells are gradually released due to the rupture of the cell walls. The release of these viscous substances in the cells will not only increase the viscosity of the fluid in the grinding chamber, but also adhere to or wrap around the surface of the agitator, grinding beads and the inner wall of the grinding chamber. The increase in the viscosity of the fluid and the accumulation of intracellular substances on the surface of the grinding beads have a lubricating and elastic shock-absorbing effect on the grinding beads, which will consume the kinetic energy of the grinding beads, thereby weakening the shearing and squeezing effect of the grinding beads on plant cells, and reducing the cell wall breaking efficiency of the bead mill. In industrial production, the large accumulation of intracellular substances in the grinding chamber causes blockage and discharge difficulties, which is not conducive to the continuous progress of the wall breaking process. Therefore, the industrial large-scale application of the bead mill method for breaking plant cells requires further improvement of the bead mill method.

[0047] The microwave method is limited to polar solvents, and the increase in temperature during the cell wall breaking process can easily damage the product. It can only be used to break the cell walls of some cells in the laboratory and is difficult to apply to industry.

[0048] Therefore, although there are many traditional cell wall disruption technologies and new technologies are constantly emerging, these technologies currently have some problems to a greater or lesser extent. Most technologies are only suitable for laboratories and are difficult to achieve large-scale industrial applications. For the research and development of efficient cell wall disruption technologies, the key factors to be considered include: process economy, industrial scalability and product quality reliability.

[0049] The present application proposes an integrated device for nano-grinding, wall-breaking, extraction and filtration using ultra-low temperature freezing-assisted high-pressure-double vortex countercurrent back-pressure cavitation continuous dynamic circulation. In the process of cell crushing using ultra-low temperature freezing-assisted high-pressure-double vortex countercurrent back-pressure cavitation continuous dynamic circulation, the viscosity of bamboo leaf liquid is reduced and cells are dispersed in the grinding liquid, the fluidity of the grinding liquid is increased, the accumulation of bamboo leaf cells and viscous substances is reduced, and the device has the function of dispersing and reducing the viscosity of organic matter and increasing the circulation of the grinding liquid. Thus, the cell wall breaking efficiency of the device is improved, while also avoiding the emulsification and destruction of useful substances released by the broken bamboo leaf cells due to long-term wall breaking. The integrated device of the present application has the functions of ultra-low temperature freezing treatment, high-pressure-double vortex countercurrent back-pressure cavitation grinding, wall-breaking and filtration to extract nano-scale bamboo leaf flavonoid compounds. These efforts can be divided into the following six strategies.

[0050] First, this application utilizes a specific size tank and ambient cryogenic grinding.

[0051] Before plants are extracted, they need to be crushed and other treatments; the purpose of crushing is to increase the specific surface area of ​​the plant, so that the plant particles can fully contact the solvent, the effective ingredients are easier to extract, and the rate of plant extraction is increased; generally speaking, the harder and more brittle the material is, the easier it is to grind and crush, but not all materials are hard and brittle at room temperature.

[0052] Therefore, in the freeze-thaw extraction process, the solution freezing process is the key link that determines the final quality of the extract; however, the current research on the freezing change process of plant grinding liquid in a low-temperature environment is not thorough enough, and there is a lack of research reports on the relationship between its freezing rate and different production process conditions.

[0053] Therefore, the present application adopts an ultra-low temperature freezing and grinding extraction process technology for the bamboo leaf grinding liquid, and uses a solution to extract the effective ingredients in the bamboo leaves, so as to retain the activity and original molecular structure of the effective ingredients as much as possible: in the ultra-low temperature freezing environment, the bamboo leaf cells swell due to water absorption, and the ice crystals formed inside the cells due to the low temperature will pierce the bamboo leaf cell membrane, destroying the original cell structure; with the grinding process in the solution environment, the dissolved substances in the bamboo leaf cells will flow into the solution, realizing the extraction process of its pharmacological molecular substances; the pharmacological activity of the bamboo leaf flavonoids will not be affected during the low-temperature freezing and thawing process, so this method improves the quality and efficacy of its preparation products.

[0054] This application collects real-time monitoring data on thermal conductivity and fusion temperature during the ultra-low temperature freezing and grinding extraction process of bamboo leaves, and constructs a numerical model; then, based on the classical theory of computational fluid dynamics, simulates and calculates the ultra-low temperature freezing and grinding extraction process of the grinding liquid under different container sizes and ambient freezing temperature conditions; through result analysis, compares the effects of different freezing container sizes and ambient freezing temperatures on their ultra-low temperature freezing and grinding extraction process, and provides an experimental data basis and theoretical analysis basis for process improvement of the ultra-low temperature freezing and grinding extraction process of bamboo leaves.

[0055] The simulated dimensions of the ultra-low temperature freezing and grinding extraction process of bamboo leaves in this application are shown in Table 1

[0056]

[0057] As can be seen from Table 1, there are large differences in the specific surface areas of containers under different size conditions. The experimental research of this application found and verified in combination with Table 1:

[0058] (1) The final freezing time of ultra-low temperature freezing grinding extraction gradually decreases with the increase of temperature difference ΔT, and is also affected by the size of the container: the larger the specific surface area, the faster the freezing speed, and vice versa; the order of freezing time from fast to slow is: D4, C3, F6, B2, A1 and E5.

[0059] (2) The specific size of the container has a more obvious restrictive effect on the freezing process of the extract:

[0060] ① Compared with the same freezing temperature difference conditions, the specific size of the container has a greater impact on the freezing process of the grinding liquid during the ultra-low temperature freezing and grinding extraction process; in the cylindrical container, the heat transfer direction of the grinding liquid has three directions: vertical axial direction, horizontal radial direction and tangential direction; it can be seen from the experiment that the temperature distribution of each circle in the horizontal tangential direction is basically the same, which shows that the heat transfer in the freezing process is mainly in the radial and axial directions; combined with the temperature results of this experiment, it can be seen that its freezing rate depends on the relative ratio between the depth of the container and the length of the radius.

[0061] ② When the depth of the container is smaller than the radius, its freezing time is determined by its axial height; conversely, its freezing time is determined by the radius of the container; at this time, under the condition that its internal volume remains unchanged, the lower the column height, the faster the freezing speed and the shorter the freezing time.

[0062] ③ When the distance ratio is smaller, the freezing time is shorter, and vice versa, the freezing time is prolonged. This shows that the heat transfer distance directly restricts the freezing process of the grinding liquid; compared with the freezing temperature of the environment and the solution, the freezing process of the grinding liquid is more affected by the container size. The container with a shorter heat transfer distance has a better freezing effect, and its influence on the freezing process of the mixed liquid is greater than that of the freezing temperature.

[0063] (3) The grinding process is affected by the temperature inside the container. The lower the temperature, the shorter the freezing time. However, the two are not in direct proportion. When the freezing temperature is greater than -50°C, the trend of increasing freezing time does not change much. At this time, the impact of freezing energy consumption on production costs should be considered.

[0064] Therefore, combined with the energy consumption of the freezing process and the actual needs of this application, the optimal freezing process conditions for the grinding liquid of this application are: cooling temperature to -15℃~-50℃, the inner radius of the container is 60mm, the depth is 938mm, the specific surface area is 0.01, and the freezing grinding time is 30~50min.

[0065] Second, this application adopts a pear-shaped tank with a special geometric structure, combined with a dual-turbine forward and reverse vortex countercurrent drive motion mode, high-pressure-dual vortex countercurrent back pressure cavitation continuous dynamic cycle nano-grinding and wall breaking. The cell wall is one of the significant characteristics of plant cells. It is composed of a layer of tough cellulose shell, etc. Its tissue structure is relatively hard and insoluble in most solvents. It has strong resistance to chemical corrosion and radioactivity. In addition, the volume of the cell is very small, and it is difficult to destroy the cell wall by general physical and chemical methods. Most of the biologically active ingredients or medicinal ingredients exist in the cells, and only a small amount exists in the intercellular space. Therefore, the cell wall of the plant is the main obstacle to the leaching of the effective ingredients inside the cell.

[0066] Due to the efficiency of cavitation generation and the difficulty of engineering application, among the four modes, acoustic cavitation and hydraulic cavitation are the hot topics of academia and industry.

[0067] At present, acoustic cavitation is usually controlled by an ultrasonic generator. The transducer transmits the acoustic energy generated by high-frequency vibration to the liquid medium. When the acoustic energy reaches a certain threshold, cavitation bubbles begin to appear in the liquid, and the cavitation effect occurs almost simultaneously. However, the cavitation efficiency does not increase with the increase of acoustic energy. Therefore, it is only effective in laboratories and small containers with limited space. However, when it is applied to pilot production or industrialization, problems such as uneven cavitation field, low cavitation efficiency, small flux, and difficulty in amplification will arise.

[0068] Hydraulic cavitation is a pressure drop generated when a fluid passes through a restricted flow area (such as a fluid flowing through a Venturi tube). When the pressure drops below the cavitation initiation pressure, the gas dissolved in the fluid will be released, and the fluid will vaporize to produce a large number of cavitation bubbles. As the cavitation bubbles continue to flow with the fluid, they will collapse when they encounter changes in the surrounding pressure. Compared with ultrasonic cavitation, hydraulic cavitation has simple equipment and low cost, and can produce large-scale cavitation fields (such as orifice plates, Venturi tubes, liquid whistles, etc.). However, the cavitation intensity of hydraulic cavitation is relatively small and the efficiency is low, which is often not enough to trigger or enhance certain physical and chemical reactions.

[0069] According to the Venturi principle, the flow surface area suddenly decreases, the flow rate increases sharply, the pressure in the flow channel is lower than the saturated vapor pressure, cavitation occurs in the liquid, and a back-pressure cavitation effect is formed; with the release of high pressure, a strong shock wave (homogeneous phase) or a high-speed jet (heterogeneous phase) will be formed in the liquid; in extraction, this strong impact flow can effectively reduce and eliminate the barrier layer between the solvent and the aqueous phase, thereby increasing the mass transfer rate; at the same time, the impact flow produces a physical shear force on the plant and animal cell tissues, causing them to deform, rupture, and release the contents, which greatly accelerates the extraction process; in addition, the air flow rate is a key parameter affecting the extraction rate, which directly affects the turbulence, collision and mass transfer between the solvent and the bamboo leaf particles; and the bubbles are generated on the container wall, and the shape of the container will also have a certain influence on the amount of bubbles generated, thereby affecting the extraction effect; therefore, the present application of double vortex countercurrent back-pressure cavitation,

[0070] By adopting twin turbine discs with different axes, the container shape is completely reformed and the air flow rate is optimized.

[0071] This experimental study found and verified that:

[0072] ⑴ When the turbine disk of the present application rotates at a high speed of 12-20m / s in both directions, two vortices form convection, thereby increasing the hydraulic shear effect, prompting the bamboo leaf particles and the grinding medium to rotate faster. Due to the two-way, opposite-direction double vortex, the bamboo leaf particles and the grinding medium in the cylinder are stirred together by the high-speed rotating disperser, forming vortex and backflow, so that the bamboo leaf particles receive more shear and friction per unit time, achieving the purpose of repeated grinding, thereby causing the bamboo leaf particles and the grinding medium in the material to produce a stronger impact force, friction, crushing force, and shearing effect on each other, dispersing, crushing, shaping, coating, modifying, deagglomerating, and homogenizing the bamboo leaf particles in the fluid; its physical grinding does not destroy the properties of the bamboo leaf material itself, and performs loose agglomeration and real grinding; achieving the purpose of accelerating the grinding of particles and dispersing aggregates, grinding into a uniform slurry, and making the discharge more uniform, thereby allowing the effective ingredients in the bamboo leaf cells to be quickly released and fully contacted with the solvent to accelerate dissolution.

[0073] ⑵ When the bamboo leaf particle material slurry enters the grinding chamber through the improved flow channel, the flow surface area suddenly decreases and the flow velocity increases sharply, causing the pressure in the flow channel to be lower than the saturated vapor pressure, resulting in the generation of a large number of cavitation bubbles and cavitation. The cavitation bubbles undergo generation, development and final explosion. When the bubbles explode, high-speed shock waves and microjets are generated, which accelerate the movement of the bamboo leaf particles, making them have a higher speed, intensifying friction and collision, improving the efficiency of crushing tiny bamboo leaf particles, and improving the crushing of bamboo leaf particles to nanometer fineness; at the same time, due to the mutual friction, collision and shearing between the grinding medium and the bamboo leaf particles, microcracks are generated in the bamboo leaf particles themselves, and cavitation bubbles are also generated in the microcracks of the bamboo leaf particles themselves. When the cavitation bubbles collapse, high-speed shock waves and microjets are generated, which can cause the microcracks to continue to expand, explode the bamboo leaf particles, and realize the crushing of the bamboo leaf particles. At the same time, it has a dispersion effect on the material and prevents the crushed bamboo leaf particles from re-aggregating.

[0074] ⑶ The turbine disk rotates to limit the flow and shear in various ways to induce cavitation, which can produce a large number of cavitation clouds. It has strong cavitation transport, low energy consumption, and high cavitation efficiency. When the cavitation bubbles encounter pressure changes in the surrounding area during further flow with the fluid, they collapse, which not only causes cell swelling or cell wall breakdown, allowing the solvent to diffuse into the interior of the bamboo leaf particles, but also improves the collision and mass transfer between the extraction solvent and the bamboo leaf particles, which can efficiently extract the total flavonoids in the bamboo leaves.

[0075] (4) Under the synergistic effect of high pressure-double vortex countercurrent back pressure cavitation in this application, the main motion form of the fluid in the entire grinding system is turbulence. The material transfer caused by the strong mixing effect of the turbulent vortex is much greater than the effect of molecular motion. The vibration effect and some secondary effects such as diffusion, crushing, chemical effect and thermal effect generated by the bamboo leaf particles and the grinding media in the cylinder can fully loosen the cell wall structure, further expand the effect of cell perforation, cause more cells to undergo irreversible breakdown, and enhance the release and diffusion of intracellular substances.

[0076] and dissolution, thereby further improving the extraction rate of total flavonoids in bamboo leaves.

[0077] ⑸ The bottom specific surface area of ​​the pear-shaped grinding and breaking extraction tank of the present application is large, the air flow rate during cavitation is large, the amount of bubbles generated per unit time on the wall of the equipment tank is large, the turbulent effect is good, and it is conducive to collision, turbulence and mass transfer; because the radius of the upper part of the equipment tank is small, the pressure on the bubbles during the rising process decreases rapidly and breaks, and the collapse of the bubbles produces cavitation, which corrodes the surface of the bamboo leaf particles, and the solvent can diffuse into the interior of the bamboo leaf particles, and the total flavonoids are transferred to the solvent; it is more effective than traditional conventional cylindrical cavitation equipment and is more suitable for industrial large-scale production.

[0078] ⑹ Due to the introduction of double vortex back pressure cavitation, the wall breaking efficiency of the pear-shaped grinding and wall breaking extraction tank of the present application is significantly improved; in the early stage of cell wall breaking, larger cells are more easily broken, and at this time the cells are mainly broken by extrusion and shearing; as the wall breaking process proceeds, cells with smaller particle sizes are more difficult to break, and shearing gradually becomes the main wall breaking mechanism; for cavitation containers of the same shape, the extraction rate when the air flow rate is 200mL / min is always greater than that when the air flow rate is 100mL / min, and when the air flow rate is 200mL / min, the extraction rate of the pear-shaped grinding and wall breaking extraction tank of the present application is always greater than that when the air flow rate is 100mL / min. The final volume is larger than that of the cylindrical cavitation container, and the total flavonoids extraction rate increases significantly from 52.20 mg / g to 76.05 mg / g. This is because the air flow rate is large, the amount of bubbles generated per unit time is large, the turbulence effect is good, and it is conducive to collision, turbulence and mass transfer; the surface of the bamboo leaf particles is corroded, the solvent can diffuse into the interior of the bamboo leaf particles, and the total flavonoids are transferred to the solvent; and when the cavitation time is increased to 70 min, the extraction rate is basically the same as that at 50 min. Therefore, the pear-shaped grinding and wall-breaking extraction tank of this application has the best wall-breaking effect when the air flow rate is 200 mL / min and the cavitation time is 50 min.

[0079] ⑺ Under higher pressure, some cell walls inside the bamboo leaves can be destroyed, accelerating the wetting and penetration process, so that the capillaries inside the tissue are filled with solvent more quickly, thereby facilitating the subsequent diffusion of solutes, forming a more concentrated extract, forming a concentration difference with the surrounding solvent, and increasing the rate of leaching.

[0080] ⑻ Not only uniform fine particles are obtained, but also the plant cell walls are destroyed; as the grinding and breaking time increases, the plant particle size becomes smaller, and eventually the grinding and breaking to D 50 =0.02~0.08μm (while the diameter of plant cell wall is only 10μm); smaller particle size can provide higher specific surface area. The increase of specific surface area accelerates the diffusion and mass transfer of total flavonoids in bamboo leaves during cavitation, thereby shortening the mass transfer path, improving mass transfer efficiency, and accelerating the diffusion and mass transfer of total flavonoids in bamboo leaves during cavitation.

[0081] ⑼ The influence of each major factor (such as stirring linear speed, grinding medium size, material-liquid ratio, grinding time, grinding medium filling rate, etc.) on the wall breaking effect of the pear-shaped grinding and wall breaking extraction tank of the present application was studied through single-factor experiments. The results showed that:

[0082] ① The size of the grinding medium is one of the important factors affecting the cell wall breaking effect; under the condition of the same grinding medium filling rate, the smaller the grinding medium size, the greater the amount of grinding media; in the pear-shaped grinding and wall breaking extraction tank of the present application with the same volume, the increase in the size of the grinding medium means a decrease in the amount of grinding media, thereby reducing the probability of collision between the grinding beads in the tank and the bamboo leaf cells, resulting in a lower cell wall breaking rate at the same wall breaking time; this shows that if the size of the grinding medium is too large, it will seriously affect the cell wall breaking effect, and smaller-sized grinding media are more likely to achieve a higher wall breaking rate more quickly; however, for the pear-shaped grinding and wall breaking extraction tank of the present application, the size of the grinding medium is not the smaller the better; the smaller the grinding medium size, the smaller the energy that a single grinding medium can carry. When the viscosity and fluidity of the bamboo leaf cell sap change, especially when the viscosity of the bamboo leaf cell sap increases significantly, the kinetic energy carried by the grinding medium is easily consumed, thereby failing to meet the energy required for cell wall breaking, resulting in a decrease in the wall breaking rate.

[0083] ② Bamboo leaf cells can break at a relatively low linear velocity, but when the stirring linear velocity is relatively low (such as 10 m / s), the cell wall breaking rate of bamboo leaf cells is also relatively low, so it takes a long time to reach a certain cell wall breaking rate; increasing the linear velocity of the agitator of the pear-shaped grinding and wall breaking extraction tank of the present application means that more and more grinding media have sufficient energy to break the cell walls, and the cell wall breaking rate will therefore increase rapidly; however, when the stirring linear velocity is too high, the cell wall breaking rate cannot increase as quickly as expected; as the linear velocity increases, the cell wall breaking rate of bamboo leaf cells increases. When the linear velocity increases to a certain extent (such as 2.3 m / s), the increase in the cell wall breaking rate becomes relatively slow. What is more disadvantageous is that a higher stirring linear velocity consumes more energy; this shows that an appropriate stirring linear velocity should be selected in the process of bamboo leaf cell wall breaking.

[0084] ③ In the early stage of bamboo leaf cell wall breaking, the pear-shaped grinding and wall-breaking extraction tank of the present application has a faster wall-breaking rate, that is, a higher cell wall-breaking rate is achieved in a very short time, for example, the cell wall-breaking rate reaches 61.7% in 5 minutes; this is because the pear-shaped grinding and wall-breaking extraction tank of the present application has a strong wall-breaking ability for cells; however, as the wall-breaking time increases, the wall-breaking rate decreases. It can be seen that at 10 minutes, the cell wall-breaking rate reaches 79.9%, which is only an increase of 18.2% compared with the wall-breaking rate at 5 minutes. The wall-breaking rate gradually slows down with the increase of time; this change, one On the one hand, this is because the number of remaining unbroken cells is decreasing, and on the other hand, the release of intracellular substances causes the viscosity and fluidity of the bamboo leaf cell fluid in the grinding chamber to change, reducing the probability of cell wall breaking; in addition, after a long period of wall breaking, the cell wall breaking rate can eventually reach a larger value, that is, the cell wall breaking rate reaches 97.4% after 45 minutes of wall breaking treatment; extending the wall breaking time means an increase in energy consumption and a reduction in production efficiency; what is more disadvantageous is that long-term grinding not only easily causes the production of too many small cell fragments, but is also not conducive to the subsequent product separation.

[0085] From the comprehensive comparison of the above three groups of optimal parameters, it can be seen that appropriately increasing the stirring linear speed, wall breaking time and grinding medium filling rate of the shaped grinding and wall breaking extraction tank of the present application, reducing the grinding medium size and appropriate material-liquid ratio are conducive to obtaining a larger cell wall breaking rate; through orthogonal experiments, comprehensively considering the cell wall breaking rate and cell slurry viscosity, the optimized wall breaking parameter combination is: that is, the linear speed is 12-20m / s, the grinding medium diameter is 0.2-0.4mm, the grinding medium filling rate is 70-80vol%, the wall breaking time is 30-50min, the material-liquid ratio is 1:20-40, the adjustment pressure is 0.5-2.5MPa, and the air flow rate is 200L / min; experiments show that under this process conditions, the bamboo leaf cell structure is severely damaged, the cell membrane shrinks, cracks appear between the cell walls, some of the cell membranes have ruptured, and "holes" appear; generally speaking, there are almost no intact cells, and the cell walls are severely damaged; the cell wall breaking rate can reach 97.4%.

[0086] Third, the present application adopts different ethanol solution concentrations to obtain the optimal extraction yield of nano-scale bamboo leaf flavonoid compounds.

[0087] Bamboo plant cells belong to large granular cell clusters. Breaking the cell wall only breaks the cell wall of the surface layer of the cell cluster. Although these intracellular components can be quickly extracted, for the inner cells and the entire cell cluster, what is more important is that the solid-liquid contact surface is increased, which accelerates the extraction and diffusion surface of the effective components in the inner cells. When a cell on the surface of the cell cluster is broken, multiple inner cells adjacent to the cell will become solid-liquid contact surface cells, and the diffusion surface area will also increase. The change in the diffusion surface area is related to the number or ratio of cells whose walls are broken; ethanol can dissolve the lipids in the cell wall and membrane, so that a large amount of cell contents can be dissolved in it and brought out, or directly penetrate from the dissolved cells, thereby achieving the purpose of extraction.

[0088] This application designed an experiment, fixed the concentration of ethanol solution, changed the extraction time, and made a single factor experiment on the change of flavonoid yield over time. The results obtained by changing the extraction time are shown in Table 2

[0089]

[0090] From the data in Table 2, we can see the changes in flavonoid yields at different extraction times:

[0091] (1) With the increase of extraction time, the yield of flavonoids gradually increased.

[0092] (2) The lower the ethanol concentration, the shorter the time to reach equilibrium. When the ethanol concentration is below 75%, equilibrium is generally reached after 30 to 40 minutes of extraction. As the ethanol concentration increases, the time required for extraction to reach equilibrium becomes longer.

[0093] (3) It can be observed in the experiment that, because chlorophyll is insoluble in water, the color of the extracted solution gradually changes from yellow-brown to dark green with the increase of ethanol concentration; if 30% ethanol solution is selected as the extraction solvent for bamboo leaf flavonoids, there is less chlorophyll in the extract.

[0094] (4) When the ethanol concentration ratio is less than 75%, the total flavonoid yield increases with the increase of ethanol concentration; when the ethanol concentration reaches 75%, the yield decreases with the continued increase of ethanol concentration; this is because the dissolution of flavonoids in ethanol solution follows the principle of like dissolves like, and the polarity of 75% ethanol concentration is similar to that of flavonoids.

[0095] Fourth, this application adopts different material-liquid ratios to demonstrate the effect of the material-liquid ratio on the extraction amount of nano-scale bamboo leaf flavonoids.

[0096] The experimental study of this application found and verified that with the continuous dynamic increase of the solid-liquid ratio of bamboo leaf samples and ethanol-water solution, the flavonoid extraction amount showed a slow growth trend, but when the solid-liquid ratio exceeded 1:40, the extraction amount had almost no significant change; this is because with the continuous dynamic increase of the solid-liquid ratio, the contact area between the material and the solvent increased, making it easier for the ethanol solution to penetrate into the bamboo leaf cells, increasing the flavonoid extraction amount; but when the solid-liquid ratio increased continuously and dynamically to a certain extent, the concentration difference between the material and the solvent boundary layer decreased, the diffusion reached equilibrium, and the content in the solution tended to be stable. Therefore, it is more reasonable to select 1:20 to 1:40 for the final solid-liquid ratio for optimization; therefore, increasing the extraction solvent multiple increases the concentration difference between the two phases, thereby increasing the diffusion power; reducing the bamboo leaf particle size shortens the diffusion path; therefore, continuously and dynamically increasing the solvent multiple and reducing the bamboo leaf particle size can both speed up the extraction process.

[0097] Fifth, the present application adopts biological flocculants to remove impurities, thereby improving the purity of bamboo leaf flavonoid compounds.

[0098] Tannin is a polyphenolic compound with an astringent taste that can produce water-insoluble precipitates with alkaloids and proteins. It is soluble in water and alcohol, but insoluble in organic solvents such as benzene and chloroform. Therefore, water or alcohol extracts often contain a large amount of tannins, which often have a great impact on the composition of bamboo leaf extracts.

[0099] This experimental study found and verified that:

[0100] The dosage of bioflocculant solution has a significant impact on the flocculation and impurity removal effect. With the increase in the dosage of bioflocculant solution, the flavonoid retention rate of the bamboo leaf extract decreases continuously, while the light transmittance shows a trend of first increasing and then decreasing. The decrease in flavonoid retention rate may be due to the fact that the addition of bioflocculant solution affects the stability of flavonoids in the extract to a certain extent, causing them to precipitate out simultaneously with macromolecular substances such as protein and tannic acid. The change in light transmittance can be explained by the following: when the amount of bioflocculant solution added is small, the bioflocculant and substances in the extract can quickly and completely form complexes, which adsorb and precipitate suspended matter in the extract, thereby improving its clarity. When the amount of bioflocculant solution is excessive, the impurities in the extract are insufficient for the bioflocculant to form complexes, and the excess bioflocculant is suspended in the solution, resulting in a decrease in its clarity. Taking into account the flavonoid retention rate and light transmittance of the bamboo leaf extract, 4 to 5 parts of 1% bioflocculant solution are the optimal dosage.

[0101] Sixth, the present application proposes an ultra-low temperature frozen pear-shaped nano-grinding, wall-breaking and extraction integrated device with filtering function for solid-liquid separation.

[0102] In the prior art, the existing grinding machine lacks the ability to grind the material after grinding.

[0103] The material is filtered. When the grinder is grinding the material, some of the material will not be completely ground into particles. If the unground material is not filtered, the quality of the material grinding will be reduced, which will affect the use of the material.

[0104] Therefore, this application proposes a pear-shaped ultra-low temperature freezing-assisted high-pressure-dual vortex countercurrent back-pressure cavitation continuous dynamic circulation nano-grinding wall-breaking extraction and filtration integrated device with filtering function. Experimental research has discovered and verified the filtration technology used in its solid-liquid separation nanofiltration layer:

[0105] (1) Rotary filtration: Due to the high-speed rotation of solids, turbulence is formed, and the shear force on the outer wall is increased by 50% compared with traditional cross-flow filtration. At the same time, the turbulent flow continuously washes the membrane surface, preventing solids from staying on the membrane disc surface, thereby effectively preventing fouling on the membrane surface and ensuring normal filtration.

[0106] ⑵ Intermittent compression motion filtration: Ultra-thin permeation distance and it is not affected by the solid content of the feed, continuous and stable filtration time is long, which means high efficiency and high yield; membrane flux does not decline, and the yield is increased several times;

[0107] ⑶ Centrifugal action: Centrifugal force is used as the driving force, and no large-flow circulation pump is needed to provide flow rate, saving energy by 60% to 80%.

[0108] ⒉ This application uses a novel ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere with a special geometric structure nanoparticle size that is modulated for the first time, and a unique magnetic structure with a closed magnetized distribution - vortex magnetic domains, thereby achieving a new and better selective separation, adsorption and effective enrichment of active substances in natural products.

[0109] Although there are many reports on the use of macroporous resins for the separation of flavonoid components, and good separation and purification effects have been achieved, and many have been applied to industrial production; however, current research is mostly focused on the separation of flavonoid components in a certain plant, with the content increase and yield as indicators, and the adsorption process conditions are examined. The screened resins and processes are only suitable for the plant, and the selected resins are different; when it is necessary to separate a new component, it takes a lot of time to re-screen the resins and explore the processes, which is time-consuming and labor-intensive; moreover, the current literature on the adsorption behavior of macroporous adsorption resins on flavonoid compounds is still incomplete, and the effects of the properties of the resins and the structure of the compounds on the adsorption process are also unclear; it has little reference value for the separation of flavonoid compounds in different plants.

[0110] Traditional magnetic nanoparticles, due to the nanosize effect, exhibit physical and chemical properties that are completely different from those of macroscopic magnetic materials. For example, they have a large specific surface area, superparamagnetic properties, the ability to form magnetic liquids, and a variety of topological magnetic structures. Combined with their easy surface functionalization, magnetic nanoparticles are used in the separation, adsorption, and effective enrichment of target objects.

[0111] However, with the increasing application, traditional superparamagnetic particles, based on their Brown-Neel relaxation heat generation

[0112] Mechanism, its magnetization intensity value and specific absorption rate value are proportional to the square of saturation, which makes traditional superparamagnetic particles have a significantly reduced separation, adsorption and effective enrichment effect of the target due to their low magnetization intensity value. If you want to improve its magnetization intensity value, you need an external alternating magnetic field with higher field strength and frequency. While the strong amplitude and high frequency external field brings a higher specific absorption rate value, its thermal effect also quickly forms a high temperature zone, making bamboo leaf flavonoids easily degraded and denatured by heat; at the same time, the transverse relaxation rate r2 of traditional superparamagnetic particles is highly dependent on the magnetic properties of the particles; for traditional superparamagnetic particles, due to the reduction of volume magnetic anisotropy and the surface spin-canting effect, the particle saturation magnetization intensity is reduced. The Ms value is low, showing a low transverse relaxation signal (r2), slow magnetic response, and it is difficult to achieve rapid and efficient separation, adsorption and effective enrichment of the target; if the surface is coated with non-magnetic modifiers, the particle concentration per unit volume will be further diluted, thereby reducing the overall magnetic performance; in addition, the traditional superparamagnetic particles are too small to be easily located and retained in the target, nor are they conducive to the effective enrichment of the separated adsorbents, and defects such as poor physical and chemical stability are becoming increasingly prominent; therefore, these shortcomings will, to a large extent, restrict and hinder the pace of application in the fields of separation, adsorption and effective enrichment of active substances in natural products, affecting and limiting the widespread application of traditional superparamagnetic particles in this regard.

[0113] Research has shown that an important indicator affecting the application effect of Fe3O4 magnetic fluid is its magnetic responsiveness; the stronger the magnetic responsiveness of the magnetic fluid, the better its separation effect and positioning ability in the magnetic field, and vice versa; the magnetic responsiveness of the magnetic material is closely related to its relative saturation magnetization intensity, and the higher the relative saturation magnetization intensity, the better the magnetic responsiveness of the magnetic material; and currently, there is little research on the influence of the properties of Fe3O4 nanoparticles on their relative saturation magnetization intensity and magnetic responsiveness.

[0114] Therefore, there is an urgent need to find a type of magnetic nanoparticles that, on the one hand, have a high saturation magnetization intensity value and, on the other hand, can form a stable magnetic fluid, so as to make up for the shortcomings of traditional superparamagnetic particles and achieve better separation, adsorption and effective enrichment of active substances in natural products.

[0115] Compared with superparamagnetic nanoparticles, there are currently few reports on the application of magnetic vortex nanoparticles in the biomedical field; the magnetic vortex nanoparticles that have been used in biomedical research are mainly developed in iron oxide particles with morphologies such as nanodisks and nanorings, while particles with other morphologies have not been reported.

[0116] This application successfully prepared and synthesized two ionic liquid-functionalized vortex magnetic nano-elliptical hollow spheres, Fe3O4@SiO2@HDI-EMIMLpro and Fe3O4@HDI-EMIMLpro, with an aspect ratio of β=1.5, an outer major axis a=90~100nm, an outer minor axis b=60~66nm, an inner major axis a=72~80nm, an inner minor axis b=48~53nm, an inner and outer diameter thickness of 9~10nm, and the best adsorption effect on flavonoids.

[0117] This experimental study found and verified that:

[0118] (1) The magnetic domain structure of the ionic liquid functionalized vortex magnetic nano-elliptical hollow ring in this application:

[0119] The nano-elliptical hollow ball of the present application forms a unique magnetic vortex structure through the interaction between static magnetic field energy and exchange energy when the magnetocrystalline anisotropy energy is negligible. The magnetic moment is distributed in a closed clockwise or counterclockwise magnetization along the surface, while at the central vortex core, the magnetic moment is distributed vertically along the surface to form a "vortex core". Due to the closed distribution of the magnetic moment, the stray field is reduced, which can effectively weaken the magnetic dipole interaction between particles, thereby avoiding the occurrence of particle agglomeration, and having the magnetic conditions for forming a stable magnetic nano-hollow ball.

[0120] It can be seen from Lorentz transmission electron microscopy observations that no matter it is a single particle or a pair or even multiple particles, they all show a magnetized vortex distribution in the remanent magnetic state. The results show that in the remanent magnetic state, the magnetic domain structure of the nano-ellipsoidal hollow sphere of the present application is a magnetic vortex domain, proving the existence of a magnetic vortex structure in the nano-ellipsoidal particles of the present application.

[0121] (2) Experimental results show that the formation of the magnetized vortex state originates from the confinement effect of the specific size and geometric morphology of the particles, which is the result of the system's total free energy in the magnet taking a minimum value at the characteristic scale. The unique vortex domain structure of the magnetic nano-elliptical hollow sphere in this application has a significant morphology-size dependence. The geometric morphology and particle size of the particles play a decisive role in the formation and stability of the magnetized vortex structure:

[0122] ① Under the same major axis a, for ellipsoidal particles with a larger minor axis b, the magnetization vortex state dominates the remanent magnetization configuration; while for ellipsoidal particles with a smaller minor axis b, in the remanent magnetization state, due to the narrower width of the particles and the stronger demagnetization energy, their remanent magnetization configuration is more likely to form a single domain distribution;

[0123] ② Under the same minor axis size b, the coercive force is smaller;

[0124] ③ For particles with the same β, as the particle size decreases, the field width of the magnetized vortex state that exists stably in an external rotating magnetic field gradually narrows;

[0125] ④ For vortex magnetic nano-elliptical hollow rings with different thicknesses and outer diameters, the size of the magnetic vortex state is the same when the inner-outer diameter ratio β=1.5: under the corresponding inner-outer diameter ratio, the vortex magnetic nano-elliptical hollow ring only forms a stable magnetic vortex structure in the inner-outer diameter surface area of ​​the vortex magnetic nano-elliptical hollow ring;

[0126] ⑤ When magnetized in an external rotating magnetic field, the magnetic vortex state of the vortex magnetic nano-elliptical hollow sphere will transform into other states, and this process is closely related to the geometric morphology of the particles;

[0127] ⑥ The elliptical hollow spherical morphology and larger particle size make it exhibit high magnetic susceptibility and magnetization intensity values, and have a faster and stronger magnetic response in a small external rotating magnetic field; at the same time, due to its larger particle size, the vortex magnetic nano-elliptical hollow spherical ball exhibits higher magnetic susceptibility and saturation magnetization intensity than traditional superparamagnetic particles.

[0128] ⑶ By modifying the surface of the vortex magnetic nano-ellipsoidal hollow sphere of the present application, its dispersibility and magnetic stability in the environment are increased. The two effects of surface effect and volume effect can be specifically reflected in the surge in the specific surface area of ​​the vortex magnetic nano-ellipsoidal hollow sphere, the increase in functional group density and selective absorption capacity, the shortening of the time to reach adsorption equilibrium, and the greatly improved stability of the vortex magnetic nano-ellipsoidal hollow sphere; not only greatly improves the problems of easy agglomeration caused by its high specific surface area, making the particles unstable, etc., thereby improving the selectivity of magnetic particles for target analytes, but also protects the vortex magnetic nano-ellipsoidal hollow sphere from being oxidized in the environmental matrix, which makes the separation and enrichment of target analytes more efficient, rapid and convenient.

[0129] (4) The addition of ionic liquids shows a strong response to the external magnetic field and has a magnetic effect, which can make the present invention

[0130] The vortex magnetic nano-elliptical hollow ball can be easily separated and magnetically guided under the action of an external rotating magnetic field; it has strong magnetism when an external rotating magnetic field is applied, and the magnetism disappears quickly when there is no magnetic field; thus, the vortex magnetic nano-elliptical hollow ball of the present application is not permanently magnetized in a magnetic field.

[0131] ⑸ When the vortex magnetic nano-ellipsoidal hollow sphere of the present application is placed in an external rotating magnetic field, the vortex magnetic nano-ellipsoidal hollow sphere of the present application itself is magnetized and a magnetic field is induced. The superposition of the two causes the magnetic lines of force near the vortex magnetic nano-ellipsoidal hollow sphere of the present application to be deformed, forming a gradient magnetic field.

[0132] ⑹ The ionic liquid functionalized vortex magnetic nano-ellipsoidal hollow spheres of the present application have hydroxyl groups, which have hydrogen bonding effects with flavonoids. At the same time, the imidazole ring has a π bond, and the five-membered ring forms a conjugation, which enhances the adsorption of flavonoids through the π-π bond effect; under the action of an external rotating magnetic field, the friction generated by the flow of the flavonoid solution will cause the vortex magnetic nano-ellipsoidal hollow spheres to be disturbed in the microenvironment, so that the vortex magnetic nano-ellipsoidal hollow spheres will cut the magnetic lines of force, and then an induced magnetic field is generated on the magnetic pipeline. The magnetic field polarity on different vortex magnetic nano-ellipsoidal hollow spheres will be different, and there will be attraction or repulsion between particles. At the same time, combined with the effects of gravity, fluid force, etc., the particles can be stably suspended, so that the gaps between the particles are increased, which is beneficial to the adsorption of the vortex magnetic nano-ellipsoidal hollow spheres of the present application.

[0133] ⑺ Bamboo leaf flavonoids have phenolic hydroxyl groups and glycoside chains, and have certain polarity and hydrophilicity. Bamboo leaf flavonoids can form hydrogen bonds with solvent molecules and flavonoid molecules themselves; when an external rotating magnetic field is applied, the action of the magnetic field polarizes the electron cloud that forms the hydrogen bond, generating an induced magnetic torque, causing the energy of the hydrogen bond to change, causing the hydrogen bond to weaken or bend, thereby reducing the viscosity of the bamboo leaf flavonoid solution and accelerating the diffusion rate, which is beneficial to improving the adsorption rate of the ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere of the present application.

[0134] 6. This application addresses the shortcomings of the single extraction method in the prior art and proposes a method for preparing an ultra-high-purity nanoscale bamboo leaf total flavonoid dispersion. Compared with other known methods, it has the following advantages:

[0135] ⑴ The first integrated device of ultra-low temperature freezing-assisted high pressure-double vortex countercurrent back pressure cavitation continuous dynamic circulation nano-grinding wall-breaking extraction and filtration is developed to extract nano-scale bamboo leaf flavonoids, which has the following advantages.

[0136] ①Compared with traditional mechanical grinding methods:

[0137] In traditional mechanical grinding methods, during the operation of the grinding equipment, the high-frequency impact and friction of the grinding balls in the ball mill can generate a large amount of heat, which increases the temperature inside the mill. The longer the grinding time, the more heat is generated. The temperature increase will affect the molecular structure of the plant material, making it easy to become soft, sticky, and deteriorate. This will not only consume part of the plant material, but also destroy the biological activity of the plant material itself.

[0138] The present application adopts an ultra-low temperature freezing solution grinding and extraction process: first, when the sample is in a low temperature state, it will cool down rapidly and become very fragile; the sample is ground into powder using ultra-low temperature freezing force, mechanical impact force, and material friction force, making it easier to break. The principle is to first freeze the material that is tough and difficult to crush at room temperature to below the brittle point, and then grind it to the required fineness in a low-temperature grinding tank, and the original components will not be destroyed; secondly, the present application will not generate high temperature during the freezing grinding process, and low-temperature freezing grinding can also be used to perform fast and pollution-free grinding of the sample; compared with traditional mechanical grinding methods, this means that the sample is more stable, will not be damaged by heat, and will retain its original molecular structure as much as possible.

[0139] ②Comparative test on particle size and thin layer chromatography with several traditional mechanical extrusion methods and steam explosion methods:

[0140] The results show that the special pear-shaped shape and specific size structure of the tank body of the present application and the synergistic effect of the dual-turbine forward and reverse vortex countercurrent drive motion mode lead to enhanced friction between the grinding media, increased impact force of the grinding media at the rounded corners of the tank body, which can significantly shorten the grinding time and concentrate the fineness distribution range of the particles; compared with traditional equipment, the nano-grinding and wall breaking results of the present application are more accurate and the material particle size distribution is more uniform; it has the advantages of grinding and wall breaking dispersion, uniform fineness, good quality, high product fineness and little effect of heat on the active effective ingredients of bamboo leaf total flavonoids; it can greatly shorten the grinding and wall breaking time and improve the grinding and wall breaking efficiency; the extraction time is short, the continuity is strong and the cost is low.

[0141] At present, most domestic companies that extract active ingredients from agricultural products use traditional single-tank extraction, and the vast majority of my country's agricultural products deep-processing companies and traditional Chinese medicine production companies basically also use single-tank extraction; the TG2022-3 ultra-low temperature freezing-assisted high-pressure-dual vortex countercurrent back pressure cavitation continuous dynamic circulation nano-grinding and wall-breaking extraction and filtration integrated device manufactured by Shandong Warner Intelligent Equipment Co., Ltd., which is authorized by the company of this application, has many advantages such as easy use, wide adaptability, and convenience for industrial production based on the analysis and organic combination of the extraction principles of each component; compared with traditional single-tank extraction equipment, it has obvious advantages and thus has a good market prospect, which provides a huge market space for the promotion and application of the extraction equipment; at the same time, the equipment also provides a certain technical theoretical basis for the development and research of natural product extraction equipment.

[0142] The process development and research work involved in this application overcomes the shortcomings of the traditional solvent method, such as large equipment investment, complex process, low yield, and difficulty in industrial production, and develops an innovative preparation, extraction and separation method with low cost, simple process, high degree of mechanization, low energy consumption, high product purity and high environmental quality.

[0143] ⑵This application adopts the first-ever modulated nanoparticle size and special geometric structure, and a new ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere with a unique magnetic structure of closed magnetization distribution - vortex magnetic domains, to establish a functionalized external rotating magnetic field pipeline method for enriching flavonoid compounds, providing a new method for enriching and separating active substances in natural products, thereby achieving new and better selective separation and adsorption, effective enrichment and biomedical application performance of active substances in natural products.

[0144] ① Compared with traditional superparamagnetic particles, based on the unique magnetized vortex domain, annular morphology and larger particle size of this application, it exhibits higher magnetic susceptibility and saturation magnetization intensity values, and has a faster and stronger magnetic response in an external rotating magnetic field of low field strength, which can significantly enhance the adsorption degree.

[0145] The comparative test results of this application show that:

[0146] The relaxation rate comparison table of the present invention's ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere and commercial superparamagnetic iron oxide under an applied rotating magnetic field of 1.5 T is shown in Table 3.

[0147]

[0148] It can be seen from Table 3 that the r2 of the ionic liquid functionalized vortex magnetic nano-elliptical hollow ring in this application * The transverse relaxation signal value is almost 4 times that of commercial superparamagnetic iron oxide, and the transverse relaxation signal r2 *The ratio of the transverse relaxation signal r1 is 2 orders of magnitude higher than that of commercial superparamagnetic iron oxide. There are two reasons for this: on the one hand, the present invention has a larger size, which results in a higher saturation magnetization, resulting in a transverse relaxation signal r2 * On the other hand, under the action of an external rotating magnetic field, the present invention will undergo a vortex magnetic morphology transformation, which will have a greater impact on the inhomogeneity of the local field around the nanoring, thereby also leading to its transverse relaxation signal r2 * The value becomes higher. This further shows that the present invention has better application advantages and potential than superparamagnetic iron oxide particles as an effective enrichment for separation and adsorption.

[0149] Second, a vibrating sample magnetometer was used to measure the hysteresis loops of conventional superparamagnetic iron oxide nanoparticles and the ionic liquid-functionalized vortex magnetic nanoelliptical hollow spheres of the present application. Comparison of the hysteresis loops of the two samples confirmed that the present application had a higher Ms value than conventional superparamagnetic iron oxide nanoparticles.

[0150] Third, the vortex magnetic nano-elliptical hollow spherical ring of the present application has nanoparticles with a magnetic vortex structure. Due to the closed distribution of magnetic moments, the stray field is reduced, which can effectively weaken the magnetic interaction between particles, thereby avoiding the occurrence of particle agglomeration and having the magnetic conditions for forming a stable magnetic sol; at the same time, due to the relatively large particle size of the present application, it exhibits a higher magnetic susceptibility and saturation magnetization intensity than superparamagnetic particles.

[0151] Fourth, loading the vortex magnetic nano-elliptical hollow spherical ball functionalized with the ionic liquid of the present application into the pipeline can increase the load capacity, increase the elution time, and make the target object more fully contact with the present application, thereby obtaining a better enrichment and separation effect, with the advantages of high separation efficiency, fast speed, large specific surface area, and strong load capacity.

[0152] ②Compared with traditional separation and purification methods, such as macroporous resins:

[0153] First, the ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere of the present application replaces the ordinary adsorption resin under the action of an external rotating magnetic field, thereby increasing the contact area between the present application and the liquid phase, and the pipeline design greatly improves the processing capacity. Coupled with the enhancing effect of the magnetic field, compared with traditional ordinary adsorption resins, the adsorption capacity of the present application for bamboo leaf flavonoids is not reduced due to magnetization treatment, and the advantages of the present application are further reflected in the treatment of turbid materials and the improvement of operating flow rate. This shows that while the present application maintains the original adsorption performance well, it takes advantage of its own advantages to appropriately relax the pretreatment conditions of the material.

[0154] Second, this application has a large specific surface area and strong load capacity, so it uses less material and occupies less space than a macroporous resin column; used ionic liquid functionalized vortex magnetic nano-elliptical hollow spheres can be recycled and reused by ultrasonic cleaning and other methods, and magnets are used to assist in the recycling process to prevent loss.

[0155] Third, the surface of the vortex magnetic nano-elliptical hollow sphere prepared in this application is modified with rich amino groups. The most significant advantage is its strong selectivity and simple operation. It can directly separate the extract from the bamboo leaf flavonoid compound solution. The entire separation process is time-saving and labor-saving, and the operation is simple and easy to control. The separation of the adsorbed extract and the original solution can be achieved by applying an external rotating magnetic field. It is a very good separation and purification method; it is expected to be applied to the extraction and separation system of flavonoids and organic acid compounds in complex component systems such as other Chinese medicinal materials.

[0156] ③Compared with the existing traditional solid phase extraction material sample pretreatment method:

[0157] First, the amount of extractant used is small and the extraction efficiency is high; the solid-phase extractants commonly used at present have large particle sizes (tens to hundreds of microns), small specific surface areas, low extraction capacities, small extraction penetration volumes and enrichment multiples; the ionic liquid-functionalized vortex magnetic nano-elliptical hollow spheres of the present application have large surface areas, high extraction capacities and strong surface adsorption forces.

[0158] Second, it is environmentally friendly; during the extraction process, only a very small amount of a single solvent is consumed, and no other toxic or harmful substances are introduced, which is environmentally friendly.

[0159] Third, the process is simple and the extraction speed is fast. On the one hand, the nanomaterial has a small particle size and a short diffusion path, resulting in a fast equilibrium speed. On the other hand, the ionic liquid-functionalized vortex magnetic nano-elliptical hollow ring prepared in this application has excellent superparamagnetism. By applying an external rotating magnetic field, the target compound and the mother liquor can be quickly and completely separated in a very short time. This overcomes the shortcomings of conventional nanomaterial solid-phase extraction, such as large column resistance and time-consuming and labor-intensive processes, making it very suitable for large-scale sample processing.

[0160] Fourth, it can extract target substances from complex actual samples without interference; its size exclusion function prevents macromolecular substances such as proteins commonly found in environmental media from entering the ionic liquid functionalized vortex magnetic nanospheres of this application, thereby affecting the extraction efficiency.

[0161] Fifth, the entire enrichment process took only 50 minutes, which is less than the 60-100 minutes required by most other methods.

[0162] min, more efficient; the results show that compared with the known reported methods, the ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere method proposed in this application is faster, more effective, more sensitive and more reliable for the separation, adsorption and effective enrichment of active substances from natural products; this separation mode is easy to operate, has high enrichment efficiency and the magnetic material is reusable, which solves the drawbacks of traditional separation methods and overcomes to a certain extent the shortcomings of general solid phase extraction stationary phases such as short service life, non-reusability and high price.

[0163] ⑶ This application utilizes Ampere's circuit theorem and Biot-Savart's law. When current passes through the conductor ring, the intensity of the magnetic field increases linearly in the direction of the symmetry axis, and then decreases linearly in the opposite direction, forming a rotating magnetic field; this rotating magnetic field will cause the conductor ring to rotate. By analyzing the motion state of the ionic liquid functionalized vortex magnetic nano-elliptical hollow spherical ring of this application under a rotating magnetic field, its performance is evaluated.

[0164] ① Under a rotating magnetic field, 67.2% of commercially available spherical magnetic composite particles agglomerate, while the ionic liquid-functionalized vortex magnetic nano-elliptical hollow spheres prepared by the present application basically do not agglomerate; due to the weak magnetic anisotropy of the spherical particles, the magnetic torque generated under a rotating magnetic field cannot reach the energy required for the particles to rotate; ② Most commercially available spherical particles cannot complete a 360° rotation independently; due to oscillation and rotation jumps, the average effective rotation frequency of the spherical particles is lower than that of the present application; as the magnetic field strength increases, the spherical particles aggregate, and the number of particles that can complete rotation independently decreases; while the present application can spin in a higher intensity magnetic field, reducing aggregation;

[0165] ③ Commercially available spherical microparticles have a higher content of magnetic material, approximately 20 times that of the present invention. This increases weight and tends to adhere to the bottom of the matrix, affecting rotational inertia. Although the present invention contains less magnetic material, its inherent magnetic anisotropy allows for superior rotational performance in a rotating magnetic field.

[0166] ④ In a low-field rotating magnetic field of different frequencies, the present application can smoothly and continuously follow the magnetic field, while spherical particles cannot rotate continuously and will oscillate back and forth, resulting in a decrease in the average effective rotation frequency; compared with commercially available spherical particles, under the same rotating magnetic field, the present application can achieve a 68% increase in the number of independent rotations; the present application has a high magnetic anisotropy, is easier to control in a low-field magnetic field, and has great application potential.

[0167] In summary, this application takes a new perspective from nanoparticles with unique vortex magnetic domain structure and proposes a new type of ionic liquid functionalized vortex magnetic nano-elliptical hollow spherical ball system. Compared with superparamagnetic nanoparticles, this application has a unique magnetization closed distribution, larger particle size and magnetization characteristics in an external rotating magnetic field, which makes it have both weak inter-particle magnetic interaction and better magnetic properties. In practical applications, it can have the advantages of superparamagnetic particles and overcome their inherent shortcomings, showing significant separation, adsorption and effective enrichment of active substances in natural products. Application performance advantages and application value. In addition, experimental studies have shown that the ionic liquid functionalized vortex magnetic nano-elliptical hollow spheres of the present application bind to specific molecules or antibodies, which can achieve targeted enrichment in vivo. Their larger particle size allows the particles to bind to more biological molecules (drug molecules, fluorescent agents, etc.), and can also achieve selective high permeability and retention (EPR) of the particles at the tumor site, which is beneficial to their enrichment in tumor tissue and improvement of tumor treatment effects; in biomedical fields such as magnetic resonance imaging, anti-tumor magnetic hyperthermia, clinical diagnosis, enzyme labeling, targeted drug carriers and magnetically controlled drug release, cell labeling and separation, regulation of gene expression, immunoassay and bioengineering (enzyme immobilization), it has shown better application advantages and potential.

[0168] As a new type of magnetic adsorbent, the ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere of this application further enriches the members and types of the "magnetic vortex nanocrystal family"; it can break the "dominant" situation of superparamagnetic nanoparticles in separation, adsorption and effective enrichment applications; at the same time, it injects fresh blood into the biomedical magnetic nanoparticle family and opens up new avenues. Due to the suitable biomedical size and good biocompatibility of this application, these research results have made preliminary magnetic mechanism exploration and paved the way for its future application in biomedicine and other fields; it can be widely used in the pre-treatment of samples such as drugs, environment, and biology.

[0169] ⑷This application is the first to obtain D 50 =0.02~0.08μm, purity 99.7~99.9% nano-level ultra-high purity bamboo leaf total flavonoids dispersion.

[0170] ① According to the Noyes-Whitney and Ostwald-Freundlich equations, when the drug particle size is reduced to the nanometer level, its surface area increases, which not only significantly increases its solubility and dissolution rate, but also makes it easier to absorb; at the same time, nanosized drugs have a bioadhesion effect, which prolongs the gastrointestinal retention time and has the possibility of multiple other absorption mechanisms, thereby significantly improving its bioavailability.

[0171] Theoretically, any particle with a nanoscale size can be called a nanomaterial. The size of nanoparticles determines their distribution and metabolic cycle in the body. Particles with a size less than 10nm have a large specific surface area and more active electrons, are highly biotoxic, and can be easily cleared by the kidneys; while particles with a size greater than 200nm will be phagocytosed by macrophages and deposited in the spleen; therefore, for considerations of bioeffectiveness and biosafety, the size of most nanomaterials currently used in the biomedical field is controlled between 10-200nm.

[0172] According to Part II of the 2005 edition of the Chinese Pharmacopoeia, 90% of the dispersed phase spherical particles in intravenous emulsion injections must be below 1 μm in size, and no spherical particles larger than 5 μm are permitted. According to the Chinese Pharmacopoeia, ultrafine powders of traditional Chinese medicines must pass through a 200-mesh sieve (with a pore size of 75 μm), while reported micropowders of traditional Chinese medicines must pass through a 300-mesh sieve (with a pore size of 47 μm). ② Based on industry consensus, the higher the purity of bamboo leaf flavonoids, the stronger their activity and the greater their polarity. To achieve effective lipid-lowering, cardiovascular disease prevention, hypoxia tolerance, and osteoporosis prevention, a purity of at least 90% is required. Therefore, purity determines the physiological activity of a drug.

[0173] ③ The research and improvement of new dosage forms of bamboo leaf flavonoids should be developed in the direction of high efficiency, rapid effect, long effect, low toxicity, easy to carry, convenient to take and easy to store; to achieve bamboo leaf flavonoids with small dosage, high absorption rate and bioavailability, and long maintenance of the necessary concentration in the body, such as micropills, dripping pills, granules, injections, sustained-release preparations, controlled-release preparations, targeted preparations, as well as new dosage forms and technologies such as granulation and tableting of bamboo leaf flavonoids whole powder without excipients.

[0174] ④ Therefore, the D prepared in the first example of this application 50 =0.02-0.08 μm, 99.7-99.9% purity, and nano-scale ultra-high-purity bamboo leaf total flavonoids dispersion. The effective ingredients are fully utilized, meeting the requirements of the above conditions, and providing a material basis for the development of new dosage forms for bamboo leaf total flavonoids. The technology overcomes the limitations of industrial bamboo leaf flavonoid extraction technology, and industrializes nano-scale ultra-high-purity bamboo leaf total flavonoids dispersion on a large scale for use in medicine, health products, special food, special functional beverages, and cosmetics as needed.

[0175] ⑷ In summary, since the content of active ingredients in most plants is low and difficult to enrich; the system is complex, large molecules and small molecules, living and non-living substances coexist, especially the existence of isomers with similar structures, separation and purification are difficult; many natural products are heat-sensitive and easily hydrolyzed, etc., which makes the products obtained by traditional extraction and separation methods have low yields, low purity, high costs, complex processes and usually residual organic solvents; therefore, it is necessary to strengthen the basic research on the extraction and separation of natural products, and develop efficient, cheap, simple and high-quality separation and extraction technologies to completely change the low-level, extensive and backward production methods of China's natural product development, which is of great significance to accelerating the process of modernization of Chinese medicine in my country; therefore, research and application of new extraction and separation methods and production models are necessary and necessary work.

[0176] However, there is currently a lack of comprehensive processing integrated technology for high-purity bamboo leaf flavonoid extracts both at home and abroad. This application innovatively proposes an ultra-low temperature freezing-assisted high-pressure-dual vortex countercurrent back pressure cavitation continuous dynamic circulation nano-grinding and wall-breaking extraction and filtration integrated device as a technology for extracting nano-scale bamboo leaf flavonoid compounds, especially the ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere combined with an external rotating magnetic field for adsorption and separation, and dynamic elution and desorption integrated technology, which solves the technical problems in the process of nano-grinding and wall-breaking extraction, separation and functional product development, and provides a basis for the industrial production of nano-scale ultra-high purity bamboo leaf total flavonoid dispersions.

[0177] Based on the technology of this application, the drug exposure of oral and non-oral dosage forms is increased, and the appropriate formulation for the most commonly used route of administration can be determined using milligram doses of the drug, providing another way to screen and identify excellent new drugs for the development of innovative drugs; the promotion and application of this model is of great significance to the material basis of the efficacy of other traditional Chinese medicines, pharmacology, prescription compatibility theory, effective quality monitoring and control, etc.

[0178] Bamboo powder is the most commonly used filler in bamboo-plastic composites. The mesh size of the bamboo powder used as a filler has a significant impact on the mechanical properties, flow properties, and microstructure of the composite. Based on the principle of fiber reinforcement, the larger the bamboo powder mesh size and the smaller the particle size, the more uniform its dispersion in the polymer matrix, and the better the mechanical properties of the composite. This is likely related to the interfacial bonding between the bamboo powder and the matrix plastic, fiber morphology, surface roughness, and internal voids. Therefore, the mesh size of the bamboo powder is a key parameter to consider in the preparation of bamboo-plastic composites.

[0179] According to reports, the highest mesh count of bamboo powder currently sold on the market is 800 mesh using German technology and 1600 mesh using Chinese technology. Therefore, research on high-mesh bamboo powder materials is still in its infancy. Due to shortcomings such as poor performance, insufficient mechanical strength, high cost, poor experience, severe operational pollution, or other reasons, it cannot simultaneously meet the requirements of safety, hygiene, environmental protection, low cost, and high mesh count. The complex production process and high preparation cost restrict its further promotion and use. So far, it has hardly been widely industrialized and put into practical commercial application.

[0180] The median particle size D 50 The solid bamboo powder precipitate with a particle size of 0.02 to 0.08 μm is powdered by spray drying and can be widely used in high value-added product fields such as construction, industry, transportation, composite materials, bioplastics, motor vehicle shells and interiors, coatings and inks, water purification, bioethanol, petrochemicals, tobacco, explosives, nanocellulose, etc., and has good economic value. DETAILED DESCRIPTION

[0181] The present application is further described in detail below through examples. These examples are only used to illustrate the present application and do not limit the scope of the present application.

[0182] Example 1

[0183] A method for preparing an ultra-high-purity nanoscale bamboo leaf total flavonoids dispersion comprises the following steps:

[0184] Step 1: Ultra-low temperature freezing assisted high pressure-double vortex countercurrent back pressure cavitation continuous dynamic cycle nano grinding wall breaking extraction and filtration integrated device to extract nano-scale bamboo leaf flavonoids:

[0185] The refrigerant ethanol is input into the jacket layer of the integrated device, the cascade ultra-low temperature freezing system of the device is started, and the cooling temperature in the pear-shaped grinding and breaking wall extraction tank is adjusted to -15°C; bamboo leaf powder and 30% ethanol solution are placed in the pear-shaped grinding and breaking wall extraction tank at a material-liquid ratio of 1:10g / mL, 5 parts of biological flocculant solution, and a grinding medium with a filling rate of 70vol% are put into the pear-shaped grinding and breaking wall extraction tank, and the double-turbine forward and reverse vortex countercurrent drive disk is turned on and rotated at a high speed of 12m / s. At the same time, the pressure pump is turned on to press the inert gas carbon dioxide into the pear-shaped grinding and breaking wall extraction tank, and the pressure is adjusted to 0.5MPa. The air flow rate is 200L / min, and the whole process is involved in ultra-low temperature continuous The dynamic cycle grinding and wall breaking / extraction process takes a total of 50 minutes. At the 15th minute of the total treatment time, the peristaltic pump is started, and a 50% ethanol solution with a material-liquid ratio of 1:10 g / mL is continuously and dynamically added dropwise within 30 minutes, eventually reaching a total processing volume of 1:20 g / mL material-liquid ratio. The pressure is then released, and the material is discharged from the discharge port of the pear-shaped grinding and wall breaking extraction tank to the solid-liquid separation nanofiltration layer, which is subjected to high-speed rotation and intermittent compression motion. Under the action of centrifugal force, the filtrate passes through the nanofiltration rotary membrane in a tangential manner under the pressure of the pump and 3 kg, and flows out from the bottom of the device through the hollow pipe. The solid-liquid separation is achieved, and the median particle size D is obtained. 50 = 0.08 μm nanoscale bamboo leaf flavonoid solution and solid bamboo powder precipitate;

[0186] Step 2: Fe3O4@HDI-EMIMLpro ionic liquid functionalized vortex magnetic nano-elliptical hollow ring combined with an external rotating magnetic field for adsorption separation and dynamic elution and desorption:

[0187] The nanoscale bamboo leaf flavonoid compound solution in step 1 and the Fe3O4@HDI-EMIMLpro ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere were mixed in a ratio of 5:1, filled in a polytetrafluoroethylene tube, ultrasonicated at 30°C for 5 minutes, and flowed through the resin column at a flow rate of 3BV / h until adsorption saturation. With the help of an annular cylindrical external rotating magnetic field close to the tube wall, the external rotating magnetic field had a magnetic induction intensity of 1T. After vortexing for 20 minutes, the external rotating magnetic field was turned off; 5BV of distilled water and 5BV of 30% ethanol were used to elute the impurities of the flavonoid adsorbent on the resin column, and then 5BV of 50% ethanol and 4BV of 70% ethanol were used to elute the flavonoids, and finally complete desorption was achieved. The total elution and desorption time was 25 minutes; the 50% and 70% ethanol eluates were combined, and then the desorbed liquid was filtered and collected;

[0188] Step 3: Low temperature vacuum evaporation and concentration:

[0189] The desorption liquid from step 2 is fed into a low-temperature vacuum evaporation and concentration device to remove water and ethanol from the desorption liquid to obtain a concentrate;

[0190] Step 4: Freeze-drying:

[0191] The concentrate obtained in step 3 was freeze-dried to obtain a particle size of D 50 =0.08μm, nano-scale ultra-high purity bamboo leaf total flavonoids dispersion with a purity of 99.7%;

[0192] The solid bamboo powder precipitate described in step 1 is dried into powder by pressure spray drying and applied in the fields of composite materials, bioplastics, motor vehicle shells and interiors, coatings and inks, water purification, bioethanol, petrochemicals, tobacco, explosives, and nanocellulose products.

[0193] Example 2

[0194] A method for preparing an ultra-high-purity nanoscale bamboo leaf total flavonoids dispersion comprises the following steps:

[0195] Step 1: Ultra-low temperature freezing assisted high pressure-double vortex countercurrent back pressure cavitation continuous dynamic cycle nano grinding wall breaking extraction and filtration integrated device to extract nano-scale bamboo leaf flavonoids:

[0196] The refrigerant ethanol was introduced into the jacket layer of the integrated device, and the cascade ultra-low temperature freezing system was started. The cooling temperature in the pear-shaped grinding and wall-breaking extraction tank was adjusted to -30°C. Bamboo leaf powder and 50% ethanol solution were mixed at a ratio of 1:15.

[0197] g / mL solid-liquid ratio, 4.5 parts of bioflocculant solution, grinding media with a filling rate of 75vol% were placed in a pear-shaped grinding and wall-breaking extraction tank, and the double-turbine forward and reverse vortex countercurrent drive disk was turned on and rotated at a high speed of 16m / s. At the same time, the pressure pump was turned on to press inert gas argon into the pear-shaped grinding and wall-breaking extraction tank, and the pressure was adjusted to 1.5MPa. The air flow rate was 200L / min, and the whole process participated in ultra-low temperature continuous dynamic cycle grinding and wall-breaking / extraction treatment, and the total time of the whole process was 40min. On the 15th of the total treatment time The peristaltic pump was started, and a 50% ethanol solution with a material-liquid ratio of 1:15 g / mL was continuously and dynamically added dropwise within 20 minutes, eventually reaching a total processing capacity of 1:30 g / mL material-liquid ratio. The pressure was then released, and the material was discharged from the discharge port of the pear-shaped grinding and wall-breaking extraction tank to the solid-liquid separation nanofiltration layer, which was subjected to high-speed rotation and intermittent compression. Under the action of centrifugal force, the filtrate passed through the nanofiltration rotary membrane in a tangential manner under the pressure of the pump and 4 kg, and flowed out from the bottom of the device through the hollow pipe. The solid-liquid separation was achieved, and the median particle size D was obtained. 50 = 0.039 μm nanoscale bamboo leaf flavonoid solution and solid bamboo powder precipitate;

[0198] Step 2: Fe3O4@SiO2@HDI-EMIMLpro ionic liquid functionalized vortex magnetic nano-elliptical hollow ball combined with an external rotating magnetic field for adsorption separation and dynamic elution and desorption:

[0199] The nanoscale bamboo leaf flavonoid compound solution in step 1 and the Fe3O4@SiO2@HDI-EMIMLpro ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere are mixed in a ratio of 5:1, filled in a polytetrafluoroethylene tube, ultrasonicated at 30°C for 5 minutes, and flowed through the resin column at a flow rate of 3BV / h until adsorption saturation. With the help of an annular cylindrical external rotating magnetic field close to the tube wall, the external rotating magnetic field has a magnetic induction intensity of 1.2T. After vortexing for 20 minutes, the external rotating magnetic field is turned off; 5BV of distilled water and 5BV of 30% ethanol are used to elute the impurities of the flavonoid adsorbent on the resin column, respectively, and then 5BV of 50% ethanol and 4BV of 70% ethanol are used to elute the flavonoids, respectively, to finally achieve complete desorption, and the total elution and desorption time is 25 minutes; the 50% and 70% ethanol eluates are combined, and then the desorbed liquid is filtered and collected;

[0200] Step 3: Low temperature vacuum evaporation and concentration:

[0201] The desorption liquid from step 2 is fed into a low-temperature vacuum evaporation and concentration device to remove water and ethanol from the desorption liquid to obtain a concentrate;

[0202] Step 4: Freeze-drying:

[0203] The concentrate obtained in step 3 was spray-freezed to obtain a particle size of D 50 =0.039μm, nano-scale ultra-high purity bamboo leaf total flavonoids dispersion with a purity of 99.8%;

[0204] The solid bamboo powder precipitate described in step 1 is dried into powder through cyclonic combined pressure spray drying and is applied in the fields of composite materials, bioplastics, motor vehicle shells and interiors, coatings and inks, water purification, bioethanol, petrochemicals, tobacco, explosives, and nanocellulose products.

[0205] Example 3

[0206] A method for preparing an ultra-high-purity nanoscale bamboo leaf total flavonoids dispersion comprises the following steps:

[0207] Step 1: Ultra-low temperature freezing assisted high pressure-double vortex countercurrent back pressure cavitation continuous dynamic cycle nano grinding wall breaking extraction and filtration integrated device to extract nano-scale bamboo leaf flavonoids:

[0208] Input refrigerant liquid nitrogen into the jacket layer of the integrated device, start the cascade ultra-low temperature freezing system of the device, adjust the cooling temperature in the pear-shaped grinding and wall-breaking extraction tank to -50°C; put bamboo leaf powder and 75% ethanol solution at a material-liquid ratio of 1:20g / mL, 4 parts of bioflocculant solution, and grinding media with a filling rate of 80vol% into the pear-shaped grinding and wall-breaking extraction tank, turn on the double-turbine forward and reverse vortex countercurrent drive disk, rotate it at a high speed of 20m / s, and start the pressure pump at the same time to press inert gas food grade 99.999% ultra-pure nitrogen into the pear-shaped grinding and wall-breaking extraction tank, adjust the pressure to 2.5MPa, and use an air flow rate of 200L / min to participate in the ultra- The low-temperature continuous dynamic cycle grinding, wall breaking / extraction treatment is carried out for a total of 30 minutes. At the 15th minute of the total treatment time, the peristaltic pump is started. Within 10 minutes, a 75% ethanol solution with a material-liquid ratio of 1:20 g / mL is continuously and dynamically added dropwise, eventually reaching a total processing volume of 1:40 g / mL. The pressure is then released, and the material is discharged from the discharge port of the pear-shaped grinding and wall breaking extraction tank to the solid-liquid separation nanofiltration layer, which is subjected to high-speed rotation and intermittent compression motion. Under the action of centrifugal force, the filtrate passes through the nanofiltration rotary membrane in a tangential manner under the pressure of the pump and 5 kg, and flows out from the bottom of the device through the hollow pipe. The solid-liquid separation is achieved and the median particle size D is obtained. 50 = 0.02 μm nanoscale bamboo leaf flavonoid solution and solid bamboo powder precipitate;

[0209] Step 2: Fe3O4@SiO2@HDI-EMIMLpro ionic liquid functionalized vortex magnetic nano-elliptical hollow ball combined with an external rotating magnetic field for adsorption separation and dynamic elution and desorption:

[0210] The nanoscale bamboo leaf flavonoid compound solution in step 1 and the Fe3O4@SiO2@HDI-EMIMLpro ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere were mixed in a ratio of 5:1, filled in a polytetrafluoroethylene tube, ultrasonicated at 30°C for 5 minutes, and flowed through the resin column at a flow rate of 3BV / h until adsorption saturation. With the help of an annular cylindrical external rotating magnetic field close to the tube wall, the external rotating magnetic field had a magnetic induction intensity of 1.5T. After vortexing for 20 minutes, the external rotating magnetic field was turned off; 5BV of distilled water and 5BV of 30% ethanol were used to elute the impurities of the flavonoid adsorbent on the resin column, and then 5BV of 50% ethanol and 4BV of 70% ethanol were used to elute the flavonoids, and finally complete desorption was achieved. The total elution and desorption time was 25 minutes; the 50% and 70% ethanol eluates were combined, and then the desorbed liquid was filtered and collected;

[0211] Step 3: Low temperature vacuum evaporation and concentration:

[0212] The desorption liquid from step 2 is fed into a low-temperature vacuum evaporation and concentration device to remove water and ethanol from the desorption liquid to obtain a concentrate;

[0213] Step 4: Freeze-drying:

[0214] The concentrate obtained in step 3 was spray-freezed to obtain a particle size of D 50 =0.02μm, nano-scale ultra-high purity bamboo leaf total flavonoids dispersion with a purity of 99.9%;

[0215] The solid bamboo powder precipitate described in step 1 is dried into powder through cyclonic combined pressure spray drying and is applied in the fields of composite materials, bioplastics, motor vehicle shells and interiors, coatings and inks, water purification, bioethanol, petrochemicals, tobacco, explosives, and nanocellulose products.

[0216] The present application has found and verified through experimental research that the purity of the product obtained according to the above embodiment 3 is 99.9%, D 50 =0.02μm nano-scale ultra-high purity bamboo leaf total flavonoids dispersion:

[0217] ⑴ Effects of bamboo leaf flavonoids samples with different purities on blood lipid levels in mice (x±s), see Table 4

[0218]

[0219] Note: The bamboo leaf flavonoids group with 50% purity on the conventional market and the bamboo leaf total flavonoids group in Example 3 of this application were both fed a high-fat diet for 5 weeks. After 5 weeks, three mice were randomly selected without fasting to draw blood and measure serum TC and TG.

[0220] As can be seen from Table 4, the TC and TGG levels of the high-fat diet group were significantly higher than those of the ordinary diet group (P<0.01), indicating that the hyperlipidemia model of mice was successfully established and that the high-fat diet can completely cause mice to suffer from hyperlipidemia; compared with the high-fat diet group and the bamboo leaf flavonoids group with a purity of 70% on the conventional market, the bamboo leaf total flavonoids group in Example 3 of the present application significantly reduced the TC and TG levels of mice (P<0.01), and blood lipids were significantly reduced; and the sample dosage of the bamboo leaf total flavonoids group in Example 3 of the present application was only 1 / 4 of that of the bamboo leaf flavonoids group with a purity of 70% on the conventional market, and the effect of reducing TC and TG was better than the latter, providing a solid theoretical and large-scale market operability basis for the preparation of high-efficiency and low-toxic lipid-lowering drugs using high-purity nano-grade flavonoid raw materials for disease prevention and treatment.

[0221] ⑵ Its surface area, dispersibility, adsorption capacity, surface activity, etc. have undergone comprehensive changes compared with the original drug; its specific surface area has been greatly increased, thereby significantly increasing its solubility and dissolution rate, making it easy to disperse and dissolve in gastrointestinal fluid, and the contact area with the gastrointestinal mucosa has become larger, and the adhesion has been enhanced, so that the nano-scale material preparation obtained in this application has a longer residence time in the digestive tract, making the absorption of the active ingredients more sufficient and complete, greatly improving the bioavailability and efficacy of the preparation obtained in this application; it can also reduce local irritation.

[0222] All of the above descriptions of specific exemplary embodiments of the present application are for the purpose of explanation and illustration; these descriptions are not intended to limit the present application to the precise form disclosed, and it is obvious that many changes and variations can be made based on the above teachings; the purpose of selecting and describing the exemplary embodiments is to explain the specific principles of the present application and its practical application, so that those skilled in the art can implement and utilize the various different exemplary embodiments of the present application and various different selections and changes; or make equivalent substitutions for some of the technical features therein; and these modifications or substitutions, and other conceivable alternatives, are all within the scope of protection of the present application, and do not cause the essence of the corresponding technical solution to deviate from the spirit and scope of the technical solutions of the various embodiments of the present application.

Claims

1. A method for preparing an ultra-high purity nano-scale total flavonoids of bamboo leaves dispersion system, characterized in that The process steps include: Step 1: Ultra-low temperature freezing assisted high pressure-double vortex countercurrent back pressure cavitation continuous dynamic circulation nano-grinding wall breaking extraction and filtration integrated device to extract nano-scale bamboo leaf flavonoids: Inject the refrigerant into the jacket layer of the integrated device, start the cascade ultra-low temperature refrigeration system, and adjust the cooling temperature in the pear-shaped grinding and wall-breaking extraction tank to -15°C to -50°C; put bamboo leaf powder, 30-90% ethanol solution, with a material-liquid ratio of 1:10-20 g / mL, together with 4-5 parts of bioflocculant solution and grinding medium with a filling rate of 70-80 vol% into the pear-shaped grinding and wall-breaking extraction tank, start the double-turbine forward and reverse two-way eddy current countercurrent drive disk, rotate at a high speed with a linear velocity of 12-20 m / s, and at the same time start the pressure pump to press inert gas into the pear-shaped grinding and wall-breaking extraction tank, adjust the pressure to 0.5-2.5 MPa, with an air flow rate of 200 L / min, and participate in the ultra-low temperature continuous dynamic cycle grinding and wall-breaking / extraction process throughout, with the total time of the whole process being 30-50 min; at the 15th minute of the total processing time of the whole process, start the peristaltic pump, and within 10-30 min, continuously and dynamically supplement and add the 30-90% ethanol solution with a material-liquid ratio of 1:10-20 g / mL in a dropwise manner, and finally reach a total processing amount with a material-liquid ratio of 1:20-40 g / mL; then relieve the pressure, discharge the material from the discharge port of the pear-shaped grinding and wall-breaking extraction tank to the solid-liquid separation nanofiltration layer, make high-speed rotation and intermittent compression movement, and under the action of centrifugal force, the filtrate passes through the nanofiltration rotating membrane in a tangential manner under the pressure of the pump and 3-5 kg, and flows out from the bottom of the integrated device through the hollow pipe to achieve solid-liquid separation; obtain a nano-scale bamboo leaf flavonoid compound solution with a median particle size D 50 = 0.02-0.08 μm and solid bamboo powder precipitate; The refrigerant is any one of 30-80% ethanol and liquid nitrogen; The grinding medium is a zirconia ball or a ceramic ball, and the diameter of the grinding medium ranges from 0.2 to 0.4 mm; The bioflocculant solution is any one of 1% gelatin solution and 1% chitosan solution; The inert gas is any one of carbon dioxide, argon, and food grade 99.999% ultrapure nitrogen; The nanofiltration rotary membrane is a microporous filter membrane with a pore size of 0.02 to 0.08 μm; Step 2: Ionic liquid functionalized vortex magnetic nano-elliptical hollow ring combined with an external rotating magnetic field for adsorption separation and dynamic elution and desorption: The nanoscale bamboo leaf flavonoid compound solution of step 1 and the ionic liquid functionalized vortex magnetic nano-elliptical hollow ball are evenly mixed in a ratio of 5:1, filled in a polytetrafluoroethylene tube, ultrasonicated at 30°C for 5 minutes, and flowed through the resin bed at a flow rate of 3BV / h until adsorption saturation. An annular cylindrical external rotating magnetic field is applied close to the tube wall, and the magnetic induction intensity of the external rotating magnetic field is 1 to 1.5T. After vortexing for 20 minutes, the external rotating magnetic field is turned off; 5BV of distilled water and 5BV of 30% ethanol are used to elute the impurities of the flavonoid adsorbent on the resin column, respectively, and then the flavonoids are further eluted with 5BV of 50% ethanol and 4BV of 70% ethanol, respectively, to finally achieve complete desorption, and the total elution and desorption time is 25 minutes; the 50% and 70% ethanol eluates are combined, and then filtered and the desorbed liquid is collected; The ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere is any one of Fe3O4@HDI-EMIMLpro and Fe3O4@SiO2@HDI-EMIMLpro; The ionic liquid functionalized vortex magnetic nano-elliptical hollow sphere is prepared by: ⑴ In a sealed reactor, Fe 3+ is used as a reactant, and phosphate and sulfate surfactants are introduced. Under high temperature and high pressure conditions, crystals precipitate due to supersaturation. PO4 3- and SO4 2- are selectively adsorbed on the crystal planes of α-Fe2O3 crystals respectively, inducing the formation of a polyhedral structure of iron oxide crystals and preferentially dissolving along the long axis direction to form a hollow structure. By adjusting the concentration of the reactants and the auxiliary magnetic field, the nanowires are aligned directionally, promoting the formation of composite particles into nano-elliptical hollow globes with an aspect ratio β = 1.5; further using the nano-elliptical hollow globes of α-Fe2O3 as a precursor, Fe3O4 vortex magnetic nano-elliptical hollow globes with good dispersibility, high phase purity and magnetic anisotropy are obtained by hydrogen thermal reduction method; (2) Using tetraethyl orthosilicate as a precursor solvent to coat a thin layer of silicon dioxide SiO2 on its surface, thereby obtaining a Fe3O4@SiO2 composite vortex magnetic nano-elliptical hollow sphere with good dispersion; ⑶ Using hexamethylene diisocyanate (HDI) as a linker, the amino acid ionic liquid 1-ethyl-3-methylimidazole L-proline salt (EMIMLpro) was modified on the surface of Fe3O4 vortex magnetic nano-ellipsoidal hollow rings and Fe3O4@SiO2 composite vortex magnetic nano-ellipsoidal hollow rings, respectively, to obtain two ionic liquid-functionalized vortex magnetic nano-ellipsoidal hollow rings, Fe3O4@HDI-EMIMLpro and Fe3O4@SiO2@HDI-EMIMLpro; the nano-ellipsoidal hollow ring with an aspect ratio β = 1.5 has an outer major axis a = 90-100 nm, an outer minor axis b = 60-66 nm, an inner major axis a = 72-80 nm, an inner minor axis b = 48-53 nm, and an inner and outer diameter thickness of 9-10 nm; Step 3: Low temperature vacuum evaporation and concentration: Input the desorbing liquid from Step 2 into a low-temperature vacuum evaporation and concentration device to remove water and ethanol in the desorbing liquid, and obtain a concentrate; Step 4. Freeze-drying: The concentrate obtained in Step 3 is freeze-dried to obtain a nano-scale ultra-high purity total flavonoids dispersion of bamboo leaves with a median particle size D 50 = 0.02 to 0.08 μm and a purity of 99.7 to 99.9%.

2. A method for preparing an ultra-high purity nano-level total flavonoids of bamboo leaves dispersion according to claim 1, characterized in that: The ultra-low temperature freezing-assisted high-pressure - double-vortex countercurrent backpressure cavitation continuous dynamic circulation nano-grinding and wall-breaking extraction and filtration integrated device described in Step 1 is composed of a pear-shaped grinding and wall-breaking extraction tank, a jacket layer, and a solid-liquid separation nanofiltration layer; The pear-shaped grinding and wall-breaking extraction tank has a double-turbine forward and reverse two-way vortex countercurrent driving motion mode, with an inner radius of 60 mm, a depth of 938 mm, and a specific surface area of 0.01 in the container; The jacket layer is provided with input and output sealing covers. An electromagnetic valve is installed on the input sealing cover. The refrigerant is directly introduced into the jacket layer through a pump body to directly cool it. After the refrigerant absorbs heat, it is discharged through the electromagnetic valve installed on the output sealing cover, so that the pear-shaped grinding and wall-breaking extraction tank containing the material is in a certain constant-temperature low-temperature environment; the temperature is externally controlled, with a temperature control accuracy of ±0.5 °C and a temperature control range of 4 to -100 °C; The solid-liquid separation nanofiltration layer has a special structure of high-speed rotation and intermittent compression motion filtration.

3. A method for preparing an ultra-high purity nano-level total flavonoids of bamboo leaves dispersion according to claim 1, characterized in that: The freeze-drying described in Step 4 is any one of vacuum freeze-drying and spray freeze-drying.

4. A method for preparing an ultra-high purity nano-level total flavonoids of bamboo leaves dispersion according to claim 1, characterized in that: The described nano-scale ultra-high purity total flavonoids of bamboo leaves dispersion has a median particle size D 50 = 0.02 - 0.08 μm and a purity of 99.7 - 99.9%; it is used in the fields of medicine, health products, special needs food, special functional beverages, and cosmetics as required.

5. A method for preparing a dispersion of ultra-high purity nano-level total flavonoids from bamboo leaves according to claim 1, characterized in that: The solid bamboo powder precipitate described in Step 1 is made into powder by pressure spray drying or swirl-flow combined pressure spray drying, and is applied to the fields of composite materials, bioplastics, outer shells and interiors of motor vehicles, coating inks, water purification, bioethanol, petrochemical industry, tobacco, explosives, and nanocellulose products.

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