WO2005056155A1 - Procede d'extraction et appareil associe - Google Patents
Procede d'extraction et appareil associe Download PDFInfo
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- WO2005056155A1 WO2005056155A1 PCT/CN2004/000161 CN2004000161W WO2005056155A1 WO 2005056155 A1 WO2005056155 A1 WO 2005056155A1 CN 2004000161 W CN2004000161 W CN 2004000161W WO 2005056155 A1 WO2005056155 A1 WO 2005056155A1
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- Prior art keywords
- extraction
- tank
- water
- liquid
- extract
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
- A23L27/11—Natural spices, flavouring agents or condiments; Extracts thereof obtained by solvent extraction
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/30—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/30—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
- A23L5/32—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation using phonon wave energy, e.g. sound or ultrasonic waves
Definitions
- the invention relates to an extraction method and a device thereof, in particular to a method and a device for extracting using a principle of non-linear vibration and critical extraction, which can be applied to the extraction of traditional Chinese medicine and plants. Background technique
- Traditional Chinese medicine is a traditional Chinese medicine. Preventing and treating diseases with traditional Chinese medicine has a long history in China.
- the World Health Organization also recommends the use of traditional Chinese medicine to countries, hoping that people can eat safe, efficient, fast-acting and convenient Chinese medicine.
- Traditional Chinese medicine has been difficult to register, legally sell and use in the international market.
- Some active substances in medicine can only extract some effective ingredients. The rest of the active ingredients are destroyed, lost or left in the residue during the production process, which not only affects the extraction rate of traditional Chinese medicine and causes environmental pollution, but also causes shortcomings such as unstable efficacy, poor product color and taste, and unstable internal quality.
- C0 2 is generally preferred for supercritical extraction. Its basic principle is: the critical temperature (Tc) of C0 2 is 31.05 ° C and the critical pressure (Pc) is 7.38 MPa. When it is above this critical point, C0 2 has both gas and Liquid dual characteristics. It is similar to gas, its viscosity is similar to gas, and it is similar to liquid. Its density is similar to liquid. It is an excellent solvent. The interactions and diffusions between the daughters dissolve many substances.
- Tc critical temperature
- Pc critical pressure
- supercritical co 2 can dissolve substances from the matrix to form a supercritical co 2 load phase, and then reduce the pressure or increase the temperature, the solubility of supercritical co 2 decreases, and these substances precipitate (resolve), and co 2 separation, so as to achieve the purpose of extraction and separation. Because different substances have different solubility in co 2 or the same substance has different dissolution conditions under different pressures and temperatures, this extraction and separation process has higher selectivity.
- supercritical CO 2 extraction also has disadvantages that are difficult to overcome.
- the cost of this extraction method is relatively high. Because 0) 2 works in a supercritical state, a high-power air compressor must be used to compress the CO 2 gas, and the entire extraction process is continued, which results in power and energy consumption. Large quantities and high costs.
- the gases under high pressure are dangerous, leading to operational safety issues.
- the solubility of supercritical co 2 is still not as large as that of liquid, which makes the production efficiency of this extraction method relatively low.
- supercritical extraction technology is more suitable for the extraction of a single component, but it cannot guarantee the extraction of a complete single component, so it is not suitable for the extraction of all components of traditional Chinese medicine or plants.
- the traditional high-temperature extraction method whether it is water extraction or alcohol extraction, will destroy some of the original active substances in the drug, and may cause some toxic and side effects.
- the supercritical extraction technology cannot guarantee the complete extraction of a single component or the extraction of a full component, so there are certain limitations in this regard.
- the purpose of the present invention is to provide an extraction method, which can extract traditional Chinese medicine or plants at normal temperature, which not only guarantees the biological activity of traditional Chinese medicine or plant components, but also can realize the extraction of almost all components of traditional Chinese medicine or plants.
- Existing extraction processes have the disadvantage of destroying the biological activity of some components or can only perform partial extraction, and can be widely applied to the extraction of effective ingredients in the fields of traditional Chinese medicine, chemical engineering, food and the like.
- the method provided by the present invention uses non-linear vibration critical extraction to promote the dissolution and emulsification of substances in water.
- the basic principle is that under a certain pressure, water will be in a critical state.
- the non-linear vibration device will cause water to fluctuate at different frequencies and with different amplitudes. Because water absorbs different substances at different frequencies, this makes it at this time.
- Water can have high solubility for different substances, not only can dissolve water-soluble substances, but also promote the emulsification of fat-soluble substances, so as to be extracted.
- the frequency range of 18KHZ-33KHz can already be used to extract almost all of the raw material components, so it can be applied to the extraction of various raw materials such as Chinese medicine (including animal drugs) and plants, and it can also be any suitable for using the present invention.
- the substances extracted by the method have a wide range of applications. Therefore, the method provided by the present invention can be applied to the preparation of traditional Chinese medicine preparations or tablets to achieve the standardization and standardization of traditional Chinese medicine, and can also be applied to the extraction of plant juices and the extraction of active ingredients of animals, which relates to traditional Chinese medicine, health products, food and Cosmetics and other industries have important practical application value.
- extraction is performed by putting water in a critical state under high pressure conditions, and the pressure can be maintained constant during the extraction process and can also be changed within a certain range.
- the high pressure is beneficial for the wall-breaking treatment of the substance, and makes the substance easy to dissolve.
- the extraction method of the present invention includes the following steps:
- the raw materials are crushed, soaked, and installed in an extraction device. Under the conditions of 25MPa-35MPa pressure and 0 ° C-50 ° C, under the condition of non-linear vibration in the frequency range of 18KHz-33KHz, extraction is performed with water as the solvent, and then the Extract containing active ingredients of raw materials.
- the crushing and soaking process of the raw materials are for the convenience of extraction.
- the crushing can be rough treatment and the size is moderate.
- the soaking time varies with the raw materials and the degree of crushing. It is advisable to completely soak the raw materials with water.
- the extraction temperature is preferably 20 ° C-50 ° C, that is, performed at a low temperature (relative to the temperature in the prior art). Because low-temperature extraction can not only ensure the biological activity of the components, but also save the traditional heat treatment process, it has certain advancement.
- the mass ratio of the raw material to the water solvent is 1: 3-5. Compared with the ratio of the raw material to the water solvent 1: 10 in the traditional water extraction method, it can save a lot of water resources during the extraction process, and save a lot of organic solvent ethanol compared to the alcohol extraction method. Use, and reduce the concentration and drying time or dealcoholization steps in subsequent processes, can greatly reduce costs.
- the extraction time is 1 to 3 hours, preferably 2 hours.
- the method of the invention adopts nonlinear vibration and critical high pressure conditions, which can greatly enhance the solubility of water and increase the extraction rate. Almost all components can be completely extracted from drugs or plants in a short extraction time, compared with the traditional long Time cooking has high extraction efficiency.
- the extract obtained by the method of the present invention has been sterilized due to nonlinear vibration and critical high pressure treatment.
- it can be directly packed in liquid, or concentrated and dried to make capsules, injections, powders, Oral liquid or other suitable packaging.
- the method of the present invention can dissolve water-soluble and emulsified fat-soluble substances, it is suitable for the extraction of various substances, that is, the raw materials can be Chinese medicine (including animal medicine) or plants, or even any substance suitable for extraction using the method of the present invention.
- the method of the present invention can not only extract almost all components of traditional Chinese medicine, but also extract the juice of plants (including fruits), the extraction of effective ingredients in animals, and can be widely used in the processing industry of traditional Chinese medicine (including health products), Chemical, food and other fields.
- Another object of the present invention is to provide an extraction device capable of performing non-linear vibration critical extraction, which includes an extraction tank having a tank body and a top cover, a sealing structure for sealing the tank body and the top cover, and A pipe interface capable of inputting water and outputting extraction liquid to the tank body; characterized in that the device also has a high pressure pump connected to the extraction tank to keep the inside of the extraction tank at a high pressure below 10 OMpa; a raw material tank and a vibration frequency are set inside the extraction tank A non-linear vibration device in the range of 18KHz-33KHz; the top cover is provided with an air outlet and a wire connection hole, the air outlet is connected to a sealing valve, and the non-linear vibration device and the non-linear vibration device can be connected through the wire connection hole.
- the external power source of the extraction tank is connected, a water supply system is connected to the pipe interface of the input water to input water to the extraction tank, a material pump and a material liquid tank are connected to the extraction tank through the pipeline interface of the extraction liquid. connection.
- the high-pressure pump is a conventionally known technology, which can maintain high pressure in the extraction tank, so that the water is in a critical state, and the non-linear vibration device in the extraction tank emits non-linear vibration when the water is in a critical state.
- the raw materials are dissolved and extracted from all components. Due to the setting of the air vents, the gas can be easily discharged and entered, so that the extraction liquid can be discharged more fully and conveniently.
- the setting of the wire connection holes can ensure sealing and insulation.
- the non-linear vibration device is connected to an external power source, so that the non-linear vibration device is directly immersed in the liquid, and then the non-linear vibration is performed.
- the non-linear vibrating device may be arranged as a string composed of a plurality of non-linear vibrators, and the axes of adjacent non-linear vibrators are perpendicular to each other on different surfaces.
- the non-linear vibrator has two ends, and the end has an output curved surface.
- a vibrating piece is provided between the two ends of the head, an insulating layer is provided outside the vibrating piece, and a wire connects the vibrating piece and the external power source of the extraction tank.
- This type of vibration device can achieve non-linear vibration of the liquid and raw materials in the extraction tank uniformly and sufficiently.
- a circulation pump for circulating the liquid in the extraction tank may be provided outside the tank body to circulate the liquid to ensure uniform and rapid extraction.
- a temperature control device is provided on the outside of the extraction tank to keep the temperature in the extraction tank at 20 ° C to 50 ° C, so as to ensure that the extraction is performed at a normal temperature range, which is more conducive to the extraction of fat-soluble substances.
- the present invention can provide a purified water system to the aforementioned device of the present invention. Therefore, another extraction device provided by the present invention further includes a water processor, a water storage tank, and a water pump for supplying water to the extraction tank. In another preferred mode of the present invention, a concentration system is provided to further concentrate the extraction liquid in the extraction tank, so as to satisfy the subsequent processing of the product.
- an ultrasonic atomization device which includes an air filter provided on the top, an atomization chamber in the middle, a gas collection chamber and an exhaust fan located below the atomization chamber, A plurality of ultrasonic generators are provided in the atomization chamber, and a liquid inlet for inputting the extraction liquid and a liquid outlet for discharging the concentrated liquid are provided on the side wall of the atomization chamber.
- Non-linear vibration conditions may be based on the aforementioned patents of the inventor to prepare a non-linear vibration device to achieve the aforementioned frequency range, which is a non-linear vibration of ultrasonic waves.
- the use of ultrasonic vibration to break materials and promote dissolution is a well-known prior art.
- High pressure is also a technology that can be achieved under existing conditions.
- the physical properties of water in the critical state are also the prior art.
- the advantage of the present invention is that using the principles of ultrasonic nonlinear vibration, critical water structure change, and supercritical extraction in the prior art, water can be used as a solvent under high pressure and normal temperature conditions to perform nonlinear vibration.
- the plant's active ingredients are extracted from almost all components, which not only retains the advantages of supercritical CO 2 extraction, but also overcomes its unsolvable defects.
- the extraction rate of the method and device of the present invention is greatly improved.
- the method and device of the invention can make water-soluble and fat-soluble components in traditional Chinese medicine or plants can be extracted with water at normal temperature, and almost all components can be extracted, thereby greatly improving product yield and resource utilization.
- the method and device of the present invention extract at normal temperature, which can perfectly preserve the effective ingredients in traditional Chinese medicine or plants without being destroyed, and is especially suitable for the extraction of those components that are highly sensitive to heat and easy to be oxidized and destroyed, while retaining the original taste of the raw materials. It overcomes the bitter taste that may be caused by carbonization of the traditional Chinese medicine prepared by the traditional Chinese medicine boiling method or water extraction and alcohol extraction heating reflux method, and has important value in practical application.
- the method and device of the present invention use water as a solvent, which can eliminate the dealcoholization process or
- the separation step from the fluid in the supercritical fluid extraction method not only reduces the production process and saves costs, but also it is impossible for the water solvent to cause any chemical change to the traditional Chinese medicine or plants, which fully guarantees that the active ingredients of the traditional Chinese medicine or plants are not damaged.
- the method and device of the present invention use water as the solvent. Compared with supercritical CO 2 , the solubility of water is much greater than super critical CO 2 , thereby improving the extraction rate and the production efficiency. Advancement.
- the method and device of the present invention use water as the solvent. Compared with supercritical CO 2 , it does not require a high-pressure air compressor to operate in the entire extraction process, saving production costs, and because of the incompressibility of water, The high-pressure treatment is far easier to compress the gas, the energy consumption is only a few tenths of the existing technology, and the entire production process is easier to operate.
- the method and device of the present invention use water as a solvent. Compared with the supercritical 03 2 extraction method, because the gas has a certain degree of danger under high pressure, the method of the present invention has more reliable safety.
- the method of the invention has a simple production process, convenient operation, saving labor and a large amount of organic solvents, and reducing pollution of the three wastes.
- the integration of charging, water feeding, extraction and concentration of the device of the present invention is not only conducive to the implementation of the GMP standard, but also has a small volume.
- the volume of the extraction tank is about 140L, which is equivalent to the output of a 1-ton tank in the existing production technology.
- the method and device of the present invention also have anti-oxidation and sterilization effects due to the critical extraction under high pressure, which is conducive to ensuring and improving product quality.
- a product comes out of an extraction tank, it can basically be used as a finished product. Subsequent concentration and drying procedures.
- the method and device of the present invention use water as the solvent, the water-soluble and fat-soluble components in the raw materials can be extracted by using non-linear vibration and critical high-pressure extraction. Therefore, a variety of raw materials can be extracted, including traditional Chinese medicine (plant medicine). And animal drugs) and plants, and even any substance suitable for extraction using the present invention.
- FIG. 1 is an assembled plan view of an embodiment of an extraction device of the present invention
- FIG. 2 is a partial sectional view of an extraction tank of an extraction device
- FIG. 3 is a top view of the extraction tank shown in FIG. 2;
- Figure 4 is a front view of the connection between the barrel and the vibrator
- Figure 5 is a sectional view of a magnetic pump
- FIG. 6 is a schematic structural diagram of a nonlinear vibration device
- FIG. 8 is a structural schematic diagram of vibration ultrasonic atomization
- FIG. 9 is a front view of the nonlinear vibration extraction device shown in FIG. 1;
- Figure 10 is a liquid chromatogram of a ferulic acid reference substance
- FIG. 11 is a liquid chromatogram of the first extraction liquid using the method and device of the present invention
- FIG. 12 is a liquid chromatogram of the second extraction liquid using the method and device of the present invention
- FIG. 13 is extraction using ethanol reflux heating method Liquid chromatogram
- Fig. 14 is a liquid chromatogram of an extract solution obtained by applying the method and the device of the present invention to extracting the drug residue, followed by water washing and alcohol extraction.
- FIG. 1 is a schematic diagram illustrating an assembly of an extraction device according to a preferred embodiment of the present invention.
- the extraction device can be roughly divided into a water supply system, an extraction system, and a concentration system.
- the device of this embodiment is set according to the GMP standard requirements.
- the water supply system provides the extraction system with water that meets the extraction requirements. It consists of a water processor 1, a water storage tank 2, a water pump 3, and so on.
- the filtering device, water sources such as tap water, etc. enter the water processor 1 through the water inlet 4 and after purification, enter the water storage tank 2, which can be input into the extraction tank 5 through the water pump 3.
- the extraction system can realize full-component extraction of the raw materials placed in the extraction tank 5 under the conditions of high pressure of 25MPa-35Mpa and nonlinear vibration in the range of 18KHz-33KHz.
- the required components are extracted to form the extraction.
- Liquid which includes an extraction tank 5 capable of withstanding a pressure of 100 MPa, a high pressure pump 6, a material pump 7, a material liquid tank 8, an inner cylinder 23, a non-linear vibration device 24 and an air compressor 32, etc.
- the high pressure pump 6 is connected to a storage tank Between 2 and the extraction tank 5, it can pump high-pressure water into the extraction tank 5, so that the pressure in the closed extraction tank 5 reaches a predetermined value.
- the extraction tank 5 is the main equipment for realizing the non-linear vibration critical extraction method of the present invention. Only when the conditions of normal temperature, high pressure and nonlinear vibration are realized in the extraction tank 5 can the raw materials placed therein be subjected to normal temperature full-component extraction. As shown in FIG. 2, its structure has a cylindrical tank body 9, a top cover 10, a sealing washer 19 and two semicircular ring-shaped clamp members 11. The two clamp members 22 are tightly connected by bolts. The tank body 9 and the top cover 10 can be fastened, so as to achieve the sealing of the extraction tank 5. In order to meet the requirements that the tank body 9 can withstand high pressure, the tank body 9 is forged with high-strength low-alloy steel and made by welding.
- the inner wall of the tank body 9 is provided with a layer of stainless steel lining 12.
- Four pipe connections N4, N5, N6 and N7 are radially symmetrically arranged near the upper and lower ends of the side wall of the tank 9; water or other liquid purified by the water supply system can be input into the extraction tank 5 through the water pump 3 through the interface N7
- the interface N6 can be used to discharge the extract.
- a tee 13 is provided on the external pipe of each interface, and a magnetic pump 14 is also provided between the two tees 13.
- FIG. 5 shows the structure of the magnetic pump 14, which can promote the extraction tank 5
- the internal high-pressure liquid circulates between the tank body 9, the connection and the external pipeline.
- the top cover 10 covers the top of the tank body 9 and is made of stainless steel, and its outer diameter is approximately equal.
- the tank body 9 is provided with an air outlet hole N1, a wire connection hole N2, a pressure gauge connection hole N3, and a lifting lug 21 located at a central portion thereof through the upper and lower surfaces thereof.
- the wire connection hole N2 can introduce external power into the extraction tank 5 through the hole under the condition of ensuring insulation and pressure tightness;
- the pressure gauge on the top cover 10 directly connects with the inside of the extraction tank 5 through the pressure gauge connection hole N3 Connected, the pressure gauge can display the pressure value inside the extraction tank 5 in real time.
- the cross section of the clamp member 11 has a side U shape, and has two ear portions 20 on the side ear portions 20.
- a through hole through which a bolt can pass is provided.
- the clamp member 11 can be radially displaced relative to the tank body 9, when the two clamps are The pieces 11 are respectively moved toward the center of the tank, and the side ears 20 are opposed to each other.
- the side ears 20 can be connected by bolts. Since the inner side has an arc-shaped groove, the top cover 10 and the tank 9 can be convexed. The blue 22 is accommodated therein, and as the bolts are tightened, the top cover 10 and the tank body 9 are sealed.
- the inner cylinder 23 is located inside the tank body 9, and its length is slightly smaller than the length of the tank depth of the tank body 9.
- Inner tube 23 It includes a bracket 25, and a filter cloth bag 26 wrapped around the outside of the bracket 25.
- the bracket 25 is made of stainless steel and has a substantially cylindrical shape.
- a hook 27 is arranged at the center of the top end, and the hook 27 is used for hanging
- the non-linear vibration device 24 ensures that the non-linear vibration device 24 is located at the center of the extraction tank 5.
- FIG. 6 shows a schematic structural diagram of a non-linear vibration device 24, which consists of a series of 12 vibrators 28 connected in sequence that can emit non-linear vibration, and a hook 27 suspended on a bracket 25
- the vibrator 28 is transversely disposed with respect to the tank 9 and the axes of adjacent vibrators 28 are perpendicular to each other. Since the non-linear vibration device 24 is directly immersed in high-pressure water, its connecting wire must ensure that Water insulation, and to ensure that it is connected to the external power source through the wire connection hole N2 on the top cover 10 under high voltage conditions, so as to achieve nonlinear vibration.
- FIG. 6 shows a schematic structural diagram of a non-linear vibration device 24, which consists of a series of 12 vibrators 28 connected in sequence that can emit non-linear vibration, and a hook 27 suspended on a bracket 25
- the vibrator 28 is transversely disposed with respect to the tank 9 and the axes of adjacent vibrators 28 are perpendicular to each other. Since the non-
- FIG. 7 shows a cross-sectional view of the vibrator 28, which includes two end portions 29 having an output curved surface, and a piezoelectric ceramic vibrating piece 31 is sandwiched between the two end portions 29.
- An insulating layer 37 is provided on the outside of the vibrating piece 31 to insulate the surrounding liquid.
- the end of the tip portion 29 is hemispherical, so that the transmission plane of the wave of the vibrator '28 can be changed to a curved surface, so that each vibration wave can reach the maximum amplitude.
- a plurality of vibrators 28 are horizontally assembled into a string-like body, the length of which is approximately equal to the internal length of the tank 9 and the adjacent vibrators 28 The different axes of the axis are perpendicular.
- the pipe interface N6 is connected to the material liquid tank 8 through the tee 13 and the material pump 7.
- the material pump 7 can pump the extraction liquid after the nonlinear vibration critical extraction into the material liquid tank 8.
- a through hole is also provided on the top cover 10 to be connected to the external air compressor 32.
- the air compressor 32 can fill the closed extraction tank 5 with a pressurized gas, and further residues in the raw materials and The extraction in the raw material gap is squeezed out by hydraulic pressure, and then extracted by the material pump 7 to improve the utilization rate of the raw materials.
- a concentration system may also be included, which can concentrate, extract, and dry the extraction solution extracted in the extraction system, thereby satisfying the requirements for subsequent processing of the product.
- an ultrasonic atomizing device 34 is used for concentration, which is connected to the material liquid tank 8 and the extract is introduced into the device. As shown in FIG.
- the main structure mainly includes an air filter 43 provided on the top of the device, an atomizing chamber 40 in the middle, a gas collecting chamber 45 and an exhaust fan 47 located below the atomizing chamber 40, and a plurality of ultra-high
- the acoustic wave generator 44 is provided on the side wall of the atomizing chamber 40 with a liquid inlet 41 for inputting the extraction liquid and a liquid outlet 42 for discharging the concentrated liquid.
- the nonlinear vibration critical extraction device of this embodiment After the nonlinear vibration critical extraction device of this embodiment is assembled, as shown in FIG. 1 and FIG. 9, all systems are collectively combined in a frame 35, and a feeding system may be additionally provided on the frame 35 to replace manual feeding. It is also possible to provide a heavy equipment on the frame 35, such as a lifting pulley set or a small crane, and an electric control cabinet 36 is provided on one side of the frame 35 to achieve centralized control of the above components.
- the device covers only 4 square meters after assembly, and is suitable for enterprises and units with high production area and energy consumption requirements.
- the systems of the device can be relatively independent and can be easily connected, the structure is simple, and the energy consumption is very low.
- the inner tube 23 When carrying out the extraction method of the present invention for extracting plants or drugs, the inner tube 23 is first placed in the tank body 9, and the inner tube 23 is structured as a bracket 25 wrapped with a filter cloth bag 26, and a hook 27 on the bracket 25 A non-linear vibration device 24 is hung from the top.
- the non-linear vibration device 24 is located at the center of the tank 9, and its wires are connected to an external power source.
- the top cover 10 is covered on the tank body 9 and the two clamp members 11 are tightly connected with bolts, so that the top cover 10 and the tank body 9 are sealed.
- the sealing valve 18 and the material pump 7 are opened, and the extraction liquid is drawn into the material liquid tank 8.
- the air compressor 32 is connected to the air outlet N1, and the pressure is charged into the extraction tank 5. The gas is extracted by the pressure of the gas from the extraction fluid remaining in the raw material and the gap between the raw materials.
- the ultrasonic atomization device of the concentration system can concentrate the extraction solution to meet the preparation or other Standard requirements.
- the extraction liquid enters the atomization chamber 40 from the feed liquid tank 8 through the liquid inlet 41, and the ultrasonic generator 44 is started, and the water in the extraction liquid is formed into a mist and volatilized. It is discharged through the exhaust fan 46, so that the extraction can be performed.
- the liquid is concentrated, and the biological activity of the extract is not affected.
- the concentrated extract is discharged through the liquid outlet 42 for packaging or other processes.
- the water pump 3 can be directly started to inject water into the tank 9 for cleaning, and the cleaned water can be discharged directly to the outside through the pipe interface.
- the device of the present invention is not limited to the above-mentioned preferred embodiments, and may be variously modified.
- a heating device is provided in the water storage tank 2 of the water supply system to make the water reach normal temperature, and under the condition that the water supply is sufficient, the water source that meets the conditions can be directly connected to the extraction system, and the water supply system can be cancelled.
- non-linear vibration devices such as mechanical or electromagnetic type and circulating pump bodies can be used to perform non-linear vibration and promote liquid circulation.
- the top cover 10 and the can body 9 are sealed in the form of a double cone seal or a flat gasket seal known in the prior art.
- other known concentration equipment can also be used to concentrate the extract, such as the membrane separation device 38.
- This embodiment takes the extraction of Angelica sinensis as an example. Since the pharmacopoeia uses the content of ferulic acid in Angelica sinensis as the evaluation standard, and ferulic acid is a fat-soluble substance, the method and equipment of the present invention are used to perform relevant control experiments, which can fully explain that the method of the present invention can not only use water as a solvent to extract water-soluble And fat-soluble components, and has a certain extraction rate, improve the utilization rate of medicinal materials or plants.
- Angelica sinensis the dried root of Angelica sinensis (Angelyca sinensis (Oliv.) Diels).
- the manufacturer of Angelica sinensis for this experiment was Hualong Chinese Herbal Pieces Factory. The specifications were decoction pieces and the batch number was 200330621. Angelica decoction pieces are coarsely crushed and set aside.
- Example 1 For the remaining drug residue in Example 1, 15 kg of a normal temperature aqueous solution was added to the extraction tank for a second extraction, the pressure was maintained at 30 MPa, the extraction temperature was appropriately raised to 30 ° C, and the extraction time was 1 hour to obtain an extract solution. It is a light orange-yellow transparent emulsion with a specific gravity of 1.000. The liquid has no bitterness and maintains the original fragrance of Angelica sinensis. It has almost no precipitation. After 2 weeks of storage, it still maintains the state of the emulsion and there is no new precipitation, indicating that Angelica sinensis The performance of the extract is very stable.
- the obtained extract was a pale orange-yellow transparent emulsion with a specific gravity of 1.002.
- the liquid had no bitterness and maintained the original flavor of angelica. There was almost no precipitation. After 2 weeks of storage, it remained in the state of emulsion and no new precipitation occurred. This shows that the performance of Angelica sinensis extract is very stable.
- Example 4 Determination of ferulic acid content in Angelica sinensis extract using the method of the present invention The detection was performed by high performance liquid chromatography provided in Appendix VI D of the Chinese Pharmacopoeia 2000 edition.
- Ferulic acid reference substance 0733-9910 (provided by China Pharmaceutical and Biological Products Testing) Finely weigh 0.0050g of ferulic acid reference substance and add methanol to make a solution containing 10 ⁇ g per 1ml. Aspirate 10 ⁇ 1 of the reference solution accurately and inject it into a high performance liquid chromatograph (STD-10Avp, Dadao, Japan) to determine the chromatogram to obtain a ferulic acid reference spectrum, as shown in FIG. 10, and the ordinate is time (Minutes), indicating that ferulic acid peaked at about 30 minutes.
- STD-10Avp high performance liquid chromatograph
- Example 2 Take the extract solution obtained in Example 1, finely suck 15ml, place it in a conical flask with a stopper, add precisely 90ml methanol solution-hydrochloric acid (100: 1) mixed solution 10ml, weigh it and sonicate for 30 minutes. Allow to cool to room temperature, weigh again, make up the reduced weight with the above mixture, filter, and take the filtrate to obtain. 10 ⁇ 1 was precisely sucked and injected into a high performance liquid chromatograph to obtain a chromatogram, as shown in FIG. 11. The digital processor of the chromatograph can calculate: 0.1803 grams of ferulic acid per kilogram of crude drug.
- Example 2 Take the extract obtained in Example 2.
- the process of detecting ferulic acid content is as described in 2) above, and the liquid chromatogram is obtained, as shown in FIG. 12. Finally calculated that 0.0577 grams of ferulic acid per kilogram of crude drug. Compared with the detection result of the extract solution of Example 1, it shows that most of the ferulic acid in the medicinal solution has been extracted after one extraction using the method of the present invention.
- This comparative example demonstrates that the traditional method of ethanol extraction uses a high ratio of ethanol to the amount of raw materials, and that the extraction solution needs to undergo a step of removing ethanol, which not only consumes a large amount of ethanol, but also has a complicated process. Due to the high temperature treatment, some of the obtained products are changed in composition, lose their activity, and produce bitter taste. The appearance and taste of the products are not as good as those obtained by the method of the present invention.
- Example 2 The drug residue after extraction was washed with water and continuously refluxed with ethanol to extract the residue remaining after extraction using the method of the present invention in Example 1. Weigh 1.35kg (phase (600g of dried medicinal materials), rinse with warm water, add 1800ml of 70% ethanol, heat under reflux and extract for 2 hours, filter, filter the filtrate to recover ethanol and concentrate to 1000ml (that is, each ml of the extract is equivalent to 0.6g of angelica decoction pieces). Yellow more transparent liquid with slight precipitation.
- the content of ferulic acid in this comparative example is higher than the ferulic acid obtained by using the method of the present invention, since the organic components in angelica include ferulic acid in addition to sodium ferulic acid, ferulic acid esters, etc.
- the reason for the high ferulic acid content of this component, which is extracted by ethanol, is that ferulic acid is generated due to degreasing of ferulic acid esters, which changes the raw material components.
- the method of the present invention uses water as a solvent, does not substantially change the raw material components, and does not destroy the biological activity of the components.
- This comparative example essentially illustrates that the traditional ethanol extraction method changes the raw material components, while the method of the present invention performs full component extraction without changing the component activity and without chemical changes.
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- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Mycology (AREA)
- Botany (AREA)
- Physics & Mathematics (AREA)
- Acoustics & Sound (AREA)
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Priority Applications (3)
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EP04716199.7A EP1704907B1 (en) | 2003-12-08 | 2004-03-02 | An extraction method and the apparatus thereof |
US10/580,061 US7892579B2 (en) | 2003-12-08 | 2004-03-02 | Plant extraction using nonlinear vibration |
JP2006543343A JP4447608B2 (ja) | 2003-12-08 | 2004-03-02 | 抽出方法及びその装置 |
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CN0310118249.4 | 2003-12-08 | ||
CNB2003101182494A CN1236836C (zh) | 2003-12-08 | 2003-12-08 | 一种萃取方法及其装置 |
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US (1) | US7892579B2 (zh) |
EP (1) | EP1704907B1 (zh) |
JP (1) | JP4447608B2 (zh) |
CN (1) | CN1236836C (zh) |
WO (1) | WO2005056155A1 (zh) |
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Also Published As
Publication number | Publication date |
---|---|
JP4447608B2 (ja) | 2010-04-07 |
EP1704907A4 (en) | 2008-09-24 |
US20070154571A1 (en) | 2007-07-05 |
EP1704907B1 (en) | 2017-02-15 |
EP1704907A1 (en) | 2006-09-27 |
JP2007516823A (ja) | 2007-06-28 |
CN1546195A (zh) | 2004-11-17 |
CN1236836C (zh) | 2006-01-18 |
US7892579B2 (en) | 2011-02-22 |
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