JP2006129714A - Method for destroying cell wall of sparassis crispa, device for the same and method for extracting active ingredient of sparassis crispa - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for destroying the cell wall of Sparassis crispa, simply operable and capable of destroying cells in a short time, a method for recovering the active ingredient of the Sparassis crispa, showing a high recovery rate and a device for destroying the cell wall of the Sparassis crispa. <P>SOLUTION: This method for destroying the cell wall of the Sparassis crispa comprises a step of substituting water at the inside of the cells of the Sparassis crispa with a medium having compatibility with both of the water and a supercritical fluid, a step of substituting at least a part of the medium in the cells with the supercritical fluid by bringing the cells in contact with the supercritical fluid and a step of decreasing pressure at once for expanding the volume of the supercritical fluid in the cell wall rapidly to destroy the cell wall. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a method for destroying the cell wall of birch moth, a device for destroying the cell wall of birch moth, and a method for extracting an active ingredient of birch.

  Many health functional foods using natural product extracts have been known. For example, Chaga, the fungal nucleus of birch oyster (Scientific name: Fuscopia Obliqua), which is a mushroom that parasitizes the trunk of birch such as white birch, is known to have antitumor action and hypoglycemic action. Various methods have also been studied.

  The extraction method of the active ingredient from the birch is generally decocted with hot water. However, since the active ingredient is present inside the cell wall, the extraction rate of the active ingredient is extremely low. Therefore, many methods are used to destroy the cell wall and increase the recovery rate of the active ingredient. Methods for disrupting the cell wall include (1) a method using a surfactant, (2) a method using an enzyme, (3) an ultrasonic crushing method, (4) a grinding method French press method, (5) a freeze crushing method, etc. It has been known. Among these, as an example using an enzyme, a method has been proposed in which sclerotia is disrupted with ultrasound, treated with protease or cellulase, and then extracted with hot water (see, for example, Patent Document 1). As a similar method, there has also been proposed a method in which a sugar-degrading enzyme such as amylase is added to birch bamboo and subjected to enzyme treatment, followed by extraction with alcohol (see, for example, Patent Document 2).

In addition to the above method, a technique using a supercritical fluid is also disclosed as a method for destroying a cell membrane or a cell wall. (For example, refer to Patent Document 3 and Patent Document 4). In the technique described in Patent Document 3, after mixing the cell culture medium and the supercritical solution, the pressure is instantaneously reduced to rapidly expand the mixed solvent that has diffused into the cell membrane. It is supposed to be destroyed. The technique described in Patent Document 4 introduces carbon dioxide in a high-pressure gas state into a suspension of animal and plant cells in the form of microbubbles, so that the carbon dioxide dissolved in the suspension is used to form lipid membranes that constitute cell membranes and cell walls. It is a technology that penetrates the heavy membrane and destroys cell membranes and cell walls.
JP 2002-262820 A JP 2004-161748 A Japanese Patent Publication No. 6-9502 JP 2002-78478 A

  The grinding method conventionally used as a cell wall crushing method is accompanied by a thermal history at the time of destruction, so that an originally effective component may be subject to thermal destruction or denaturation. Moreover, the technique described in Patent Document 1 makes the specimen into fine particles of 10 μm or less by treating with ultrasonic waves, and further improves the solubility in a solvent by hydrolyzing proteins and the like by an enzymatic action, thereby efficiently making active ingredients. However, it requires many steps and operations for extraction, and requires much time for extraction. In the technique described in Patent Document 2, alcohol is extracted after pulverizing a specimen and a saccharide-degrading enzyme such as amylase is added for hydrolysis. Moreover, since the technique of patent document 1 and patent document 2 also uses an enzyme, there exists a possibility that these may exert an undesired influence.

  Although the method using the supercritical technology described in Patent Document 3 and Patent Document 4 has few processing steps and a relatively short processing time, even if these technologies are used to destroy plant cell bodies such as birch moss, The solubility of carbon dioxide in intracellular water is slight even in the supercritical pressure state, and cell destruction as expected is not observed.

  An object of the present invention is to provide a method for destroying the cell wall of birch moth, which is easy to operate and capable of cell destruction in a short time, a method for collecting an active ingredient of birch moth that has a high recovery rate of the active ingredient, and a device for destroying the cell wall of birch moth There is to do.

  The inventor utilizes that the carbon dioxide liquid is almost incompatible with water, but is compatible with ethyl alcohol and acetic acid, and at the same time, ethyl alcohol and acetic acid are compatible with water, A part or most of the water in the cell is once replaced with a medium compatible with water such as ethyl alcohol or acetic acid, and then pressurized with a carbon dioxide fluid in a supercritical state. By substituting a part or most of it with carbon dioxide fluid, the concentration of carbon dioxide in the cell is greatly increased, and then sudden volume expansion is caused by reducing the pressure rapidly to make carbon dioxide gaseous. Thus, a method for breaking the cell wall was found.

That is, the present invention comprises the step of replacing the intracellular water of the birch bamboo with a medium compatible with both the water and the supercritical fluid;
Replacing at least a portion of the medium in the cell with a supercritical fluid by contacting the birch salmon that has replaced the intracellular water with the medium with a supercritical fluid;
Reducing the pressure at once, and rapidly expanding the supercritical fluid in the cell wall to destroy the cell wall;
It is a method for destroying the cell wall of Birch fungus, characterized in that

  Also, in the present invention, the supercritical fluid is carbon dioxide, and the medium contains at least one of ethyl alcohol and acetic acid. Is the method.

  In addition, the present invention relates to a method for extracting an effective component of birch salmon, which comprises destroying the cell wall of birch salmon and extracting the active component from the birch salmon that has destroyed the cell wall by the method for destroying cell walls of birch salmon according to claim 1. It is.

The present invention also includes the step of replacing the intracellular water of the birch moth with a medium compatible with both the water and the supercritical fluid;
Replacing at least a portion of the medium in the cell with a supercritical fluid by contacting the birch salmon that has replaced the intracellular water with the medium with a supercritical fluid;
Reducing the pressure at once, and rapidly expanding the supercritical fluid in the cell wall to destroy the cell wall;
Extracting an active ingredient from the birch salmon that has destroyed the cell wall,
A method for extracting an active ingredient of birch moss, wherein the step of destroying the cell wall and the step of extracting the active ingredient from the birch moss that has broken the cell wall are carried out substantially in the same container.

The present invention includes a supercritical fluid forming means capable of forming a supercritical fluid;
The birch oyster mushroom, a medium compatible with both water and supercritical fluid, and a treatment tank for destroying the cell wall of birch moth mushroom that can accept the supercritical fluid;
A pressure reducing means capable of reducing the pressure in the treatment tank at once,
It is a device for destroying the cell wall of Birch fungus, characterized by comprising

  In this method, the water in the cell of the birch is replaced with a medium compatible with both water and the supercritical fluid, and the water in the cell is replaced with the medium. After the contact, at least a part of the medium in the cell is replaced with a supercritical fluid, and the cell wall is destroyed by reducing the pressure all at once. it can.

  In addition, the intracellular water of the birch moth is replaced with a medium that is compatible with both water and the supercritical fluid, and the intracellular medium is obtained by contacting the birch moss that has been substituted with the medium with the supercritical fluid. Since at least a part of the supercritical fluid is replaced with a supercritical fluid, the solubility of the supercritical fluid in the medium is very high, unlike the conventional cell wall destruction method using a supercritical fluid. As a result, the cell wall can be reliably destroyed by reducing the pressure all at once. Moreover, there is no possibility that foreign matter is taken in unlike the method using a surfactant or an enzyme.

  Further, according to the present invention, since the supercritical fluid is carbon dioxide, the critical temperature and the critical pressure are relatively low, and it is easy to form a supercritical state. In addition, since the supercritical fluid is carbon dioxide, the critical temperature is low, and the active ingredient contained in the birch is not subject to thermal denaturation. In addition, since the supercritical fluid is carbon dioxide, it is a gas at room temperature and atmospheric pressure, and can be easily removed from birch.

  According to the present invention, the medium compatible with both water and the supercritical fluid is inexpensive because it is at least one of ethyl alcohol and acetic acid. Further, since the medium is at least one of ethyl alcohol and acetic acid, it is highly compatible with water or carbon dioxide in a supercritical state. In addition, since no enzyme or the like is used, the extract is not affected. In the case of ethyl alcohol, it is safe even if it remains in the birch bamboo.

  In addition, the method for extracting the active ingredient of the present birch is a method for extracting the active ingredient from the birch salmon that has destroyed the cell wall by the above-described method for destroying the cell wall of the birch, and the active ingredient is extracted from the birch The rate is high. In addition, since the cell wall of the birch is already destroyed before the extraction operation, various extraction methods such as extraction with water and extraction with alcohol can be adopted, and options for extraction methods of active ingredients are expanded.

  Further, the method for extracting the active ingredient of the present birch bamboo includes the step of destroying the cell wall of the birch bamboo and the step of extracting the active ingredient from the birch bamboo that has destroyed the cell wall, and these steps are carried out substantially in the same container. Effective components can be extracted from birch salmon efficiently in a short time.

  Further, according to the present invention, the present cell wall disrupting device comprises a supercritical fluid forming means capable of forming a supercritical fluid, birch bamboo, a medium compatible with both water and supercritical fluid, and the supercritical fluid. Since it includes a treatment tank that breaks the cell wall of possible birch, and a pressure reducing means that can reduce the pressure in the treatment tank all at once, the cell wall of the birch can be broken using this apparatus.

  FIG. 1 is a diagram showing a schematic configuration of a cell wall destruction apparatus 1 for birch moss as one embodiment of the present invention. This embodiment will be described using oxygen dioxide as a supercritical fluid. Needless to say, the supercritical fluid is not limited to oxygen dioxide as described later. The cell wall disrupting apparatus 1 is a processing tank 10 that receives birch salmon, which is a raw material, a medium compatible with both water and supercritical fluid, and a supercritical fluid, and destroys the cell wall of birch salmon by an operation described later. Supercritical fluid supply means 20 for forming and supplying a supercritical fluid to 10, pressure adjusting means 30 for maintaining or reducing the pressure of the processing tank 10, and recovery means 40 for recovering distillate accompanying the pressure lowering operation of the processing tank 10 Is the main component.

  The processing tank 10 is a metal pressure vessel that accepts birch bamboo, which is a raw material, and has a structure that can be opened and closed so that the raw material can be accepted. A pipe line 11 for receiving the supercritical fluid is connected to the upper part, and the supercritical fluid supplied from the supercritical fluid supply means 20 is received through the pipe line 11. The pipe 11 is also used as a pipe for discharging the supercritical fluid in the processing tank.

  The processing tank 10 is installed in the thermostat 12 and is maintained at a constant temperature. The thermostatic bath 12 includes an electric heater 13 therein, and the thermocouple 14 and the temperature control device 15 that measure the temperature in the bath keep the temperature in the thermostatic bath constant. For example, when carbon dioxide is used as the supercritical fluid, since the critical temperature of carbon dioxide is 304.2K, the constant temperature bath 12 is required to have the ability to heat to this temperature or higher. In addition, a fan 16 is attached to the thermostat 12 in order to eliminate the temperature distribution of the thermostat 12. Thereby, the supercritical fluid supplied to the processing tank 10 can be stably held in a supercritical state. In this embodiment, although the example which uses the thermostat 12 is shown, a form will not be ask | required if it is provided with the function which can hold | maintain the temperature of a processing tank uniformly. For example, a water bath provided with a temperature control mechanism, an oil bath, or a ribbon-shaped electric heater or mantle heater that can be used by being attached to a treatment tank may be used.

  The supercritical fluid supply means 20 supplies a supercritical fluid to the processing tank 10, pressurizes the liquid carbon dioxide cylinder 21, which is a carbon dioxide supply source for forming the supercritical fluid, and supplies the liquid carbon dioxide to the processing tank. The main components are the supply pump 22 and the heat exchanger 24 that heats the liquid carbon dioxide fed from the supply pump 22.

  A conduit 23 is connected to the outlet of the liquid carbon dioxide cylinder 21 which is a supply source of liquid carbon dioxide, and the liquid carbon dioxide is supplied to the supply pump 22 through the conduit 23. Since the heat is generated when the supply pump 22 is moved, it is desirable to mount a cooler in the middle of the pipe line 23 to cool the liquid carbon dioxide fed to the supply pump 22 and send it. The supply pump 22 raises the liquid carbon dioxide sent to a predetermined pressure. A pipe 25 is connected to the outlet of the supply pump 22, and a pressure detector 26 that detects the pressure in the pipe is provided in the middle of the pipe 25. The operation of the supply pump 22 is controlled by the pressure detector 26 and a pressure control device (not shown).

  The pressurized liquid carbon dioxide is sent to the heat exchanger 24 installed in the thermostatic bath through the pipe 25, where it is heated to a predetermined temperature and becomes a supercritical state. Carbon dioxide in the supercritical state passes through a pipe line 27 connected to the heat exchanger 24, a gate valve 28 connected to the pipe line 27, a pipe line 29 connected to the gate valve 28, and a pipe line 11 connected to the pipe line 29. It is sent to the treatment tank 10. In the present embodiment, the pressure detector 26 and the pressure control device (not shown) are linked to the supply pump to control the pressure constant. However, the method for controlling the outlet pressure of the supply pump 22 to be constant is described below. It is not limited to this. For example, a method may be used in which a relief valve is provided at the outlet of the supply pump 22 and when the pressure rises, the carbon dioxide is returned to the pipe line 23 through the relief valve.

  In addition to the above method, supercritical carbon dioxide can be formed by the following method. From the volume of the processing tank 10 and the density of the carbon dioxide in the supercritical state, the amount of liquid carbon dioxide filled in the processing tank 10 is calculated. After liquid carbon dioxide having a critical temperature corresponding to this amount or less is sent to the treatment tank 10, the liquid carbon dioxide is heated in the treatment tank 10 to form a supercritical fluid. When this method is adopted, the heat exchanger 24 is not always necessary.

  The pressure adjusting means 30 keeps the pressure in the processing tank 10 constant or reduces the pressure as necessary, with the gate valve 31 as a main component. When the supercritical fluid supplied to the processing tank 10 is discharged, the gate valve 31 is opened through the pipe line 11 and the pipe line 32 connected to the upper part of the processing tank 10. The gate valve 31 is also a pressure reducing means having a function capable of reducing the pressure in the processing tank 10 at once as described later. A pressure detector 34 is provided through a branch pipe 33 in the pipe line 32 connected to the gate valve 31, whereby the pressure in the processing tank 10 can be detected. When the supercritical fluid is discharged through the gate valve 31, the gate valve 31 is cooled along with the adiabatic expansion, so that the fluid may solidify and close. Therefore, it is desirable to install the gate valve 31 in the thermostat 12.

  A pipeline 35 is connected to the outlet of the gate valve 31, and the pipeline 35 is connected to a collection tank which is a collection means 40 for collecting distillate. A vent pipe 41 is connected to the upper part of the recovery tank 40, and carbon dioxide discharged from the processing tank 10 is finally discharged through the vent pipe 41. Further, the recovery tank 40 is provided with a pipe line 42 and a valve 43 for discharging a distillate accompanying and distilling with the discharged carbon dioxide at the bottom.

  Next, a procedure for crushing the cell wall of birch moth using the cell wall disrupting apparatus 1 and a method for extracting an active ingredient of birch moth are described. FIG. 2 is a flowchart showing a procedure for crushing the cell wall of birch moth using the cell wall disrupting apparatus 1 and a procedure for extracting an active ingredient using the birch moth that has broken the cell wall. This flowchart only shows an example of the procedure, and it goes without saying that the operations from step S1 to step S6 may be changed and used.

  First, in step S1, the birch moth, which is a sample, is dried to reduce the amount of water contained in the sample. Since the present invention replaces the water contained in the birch cells as described later with a medium compatible with both water and supercritical fluid, it is preferable that the sample contains less water. Since drying is performed to facilitate replacement of water and the medium, the drying step may be omitted when the amount of water in the sample is small. Even when the sample contains a relatively large amount of water, the drying step can be omitted by increasing the amount of the medium or by increasing the immersion time of the sample in the medium.

  For the extraction of the active ingredient of the birch moth, it is preferable that chaga, which is a mycelium, contains a large amount of the active ingredient, but the fruit body or mycelium of the birch moth can also be used. These can of course be used alone, but fruit bodies, mycelium and mycelium may be mixed. In addition, it is needless to say that cultivated or cultured can be used for birch moths other than natural products.

  Next, in step S2, the sample is pulverized and filled into the processing tank 10. By crushing the sample, it becomes easy to replace the moisture in the sample with a medium compatible with both water and the supercritical fluid. Although the degree of pulverization is not particularly limited, the smaller the particle size, the easier the replacement of water and medium. Further, the type of pulverizer used for pulverization is not particularly limited.

  Next, in step S3, ethyl alcohol is added to the treatment tank 10, and the sample is immersed in ethyl alcohol. Ethyl alcohol is a medium that is compatible with both water and carbon dioxide, which is a supercritical fluid. By immersing a sample in ethyl alcohol, intracellular moisture can be replaced with ethyl alcohol. Although ethyl alcohol is used in the present embodiment, the medium that replaces intracellular water is not limited to ethyl alcohol. This medium may be any medium that is compatible with both water and the supercritical fluid. Therefore, if carbon dioxide is used as the supercritical fluid, methyl alcohol, a mixture of methyl alcohol and ethyl alcohol, acetic acid Can be used. Furthermore, it is also possible to use methyl alcohol, ethyl alcohol, a mixture of methyl alcohol and ethyl alcohol, and a mixture of acetic acid and water. However, since the medium is intended to replace the intracellular moisture, it is natural that the concentration of water contained in the medium is desirably low. The supercritical fluid is not limited to carbon dioxide. For example, a hydrocarbon such as propane can be used.

  In addition, when replacing intracellular water with a medium such as ethyl alcohol, it is also preferable to pressurize appropriately in the range of normal pressure to supercritical pressure using carbon dioxide or the like to be subsequently used in order to promote the replacement. Is the method.

  The immersion in ethyl alcohol in step S3 is to replace the water in the cell wall with ethyl alcohol. At this time, after sufficient immersion, the excess ethyl alcohol is excluded from the system, so that it is also possible to obtain a dry cell disruption product by subsequent cell disruption with a supercritical fluid. That is, when the supercritical carbon dioxide is rapidly released, ethyl alcohol dissolved in the carbon dioxide is accompanied and discharged out of the system, so that it is possible to obtain the remaining cell destruction product in a dry state.

  Next, in step S4, a supercritical fluid is supplied to the processing tank 10. The supercritical fluid is sent from a carbon dioxide cylinder 21 filled with liquid carbon dioxide to a supply pump 22 via a pipe line 23, boosted to a predetermined pressure by the supply pump 22, and heated to a predetermined temperature by the heat exchanger 24. It can be formed by heating. Prior to sending the supercritical fluid to the processing tank 10, the processing tank 10 is heated to a predetermined temperature.

  By supplying supercritical carbon dioxide to the treatment tank 10, the supercritical carbon dioxide is dissolved in intracellular ethyl alcohol, and at least a part of the ethyl alcohol is replaced with supercritical carbon dioxide. In order to more reliably dissolve supercritical carbon dioxide in intracellular ethyl alcohol, a method of discharging supercritical carbon dioxide supplied to the treatment tank 10 and supplying supercritical carbon dioxide to the treatment tank 10 again can be used. Good. The supercritical fluid in the present invention refers to a state where the critical temperature and the critical pressure are exceeded, and in the case of carbon dioxide, it refers to a state where the pressure exceeds 7.37 MPa and the temperature exceeds 304.2K. If carbon dioxide is used, a supercritical state can be formed at a relatively low temperature and pressure, so that the specifications of the apparatus are gradual and the apparatus cost can be reduced.

  After supplying supercritical carbon dioxide to the processing tank 10, the gate valve 31 is opened in step S5, and the pressure in the processing tank is rapidly released. As a result, the carbon dioxide in the supercritical state dissolved in ethyl alcohol in the cells of the birch tree is gasified at once and volume expansion occurs. This volume expansion destroys the cell wall of the birch moth. As described above, in the present invention, after replacing the intracellular water of the birch moss with ethyl alcohol compatible with supercritical carbon dioxide, the supercritical carbon dioxide is dissolved in the ethyl alcohol in the cell. The amount of lysis is very large, and the cell wall can be reliably destroyed by releasing the pressure.

  In the conventional cell wall destruction using supercritical fluid, a compatible medium is not interposed in both water and supercritical fluid. For this reason, supercritical carbon dioxide is dissolved in intracellular water, but even in the case of carbon dioxide in a supercritical state, the amount dissolved in water is several percent with respect to water. On the other hand, the amount of supercritical carbon dioxide dissolved in ethyl alcohol is several tens of times that of water. On the other hand, in the atmospheric pressure state, supercritical carbon dioxide is in a gas state, and the amount dissolved in ethyl alcohol is very small. By releasing the pressure of the carbon dioxide in the supercritical state, the carbon dioxide in the supercritical state dissolved in the ethanol in the birch oyster mushroom is gasified at once and causes volume expansion.

  Carbon dioxide in a supercritical state has a density that approximates that of liquid carbon dioxide, and shows the diffusion rate of carbon dioxide gas. Therefore, the use of carbon dioxide in cells is preferable because it diffuses well. However, even in the case of subcritical carbon dioxide, the amount of dissolution in ethyl alcohol is larger than the amount of supercritical carbon dioxide dissolved in water. Therefore, a subcritical fluid can be used for cell wall destruction as needed. Here, the subcritical state means that the temperature and pressure are near the critical point, or at least one of the temperature and pressure exceeds the critical point and the other is near the critical point.

  As described above, in the operation from step S1 to step S5, the cell wall of the birch tree can be reliably destroyed. In this way, the cell wall of the birch moth can be destroyed by a simple operation and in a short time. Further, the active ingredient may be extracted from the birch moss using the birch moss that has destroyed the cell wall (step S6). The fact that it is possible to extract a larger amount of the active ingredient than that of the birch that does not destroy the cell wall is shown in the demonstration data of the examples described later. Solvent extraction can be used for extraction. The solvent used for extraction of this active ingredient is not particularly limited, and water, alcohol, and the like can be used. When performing alcohol extraction, it is preferable from the viewpoint of safety to use ethyl alcohol.

  The extraction of the active ingredient with the solvent can be performed by introducing the extraction solvent into the treatment tank after the cell wall destruction in step S5 is completed. It is also possible to collect the birch salmon that has undergone cell wall destruction in step S5 from the treatment tank and extract the active ingredient using another extraction device. As described above, the extraction of the effective component of birch bamboo can be performed in the treatment tank 10 in which the cell wall is destroyed following the cell wall destruction operation, so that no special apparatus is required for extracting the effective component.

  As another embodiment of the present invention, cell wall destruction of birch moss and extraction of effective components of birch moss can be performed substantially the same. In the operation procedure shown in FIG. 2, the amount of ethyl alcohol added to the processing tank 10 is increased in step S3, and the operations in steps S4 and S5 shown in FIG. Most of the ethyl alcohol in the treatment tank is distilled with the carbon dioxide in the decompression operation in step S5, but by increasing the amount of ethyl alcohol filled in the treatment tank in step S3, Part of ethyl alcohol remains. This remaining ethyl alcohol serves to extract active ingredients from the birch moth that has broken the cell wall.

  In step S5, ethyl alcohol that is distilled with carbon dioxide may contain an active ingredient of birch salmon, so that ethyl alcohol remaining in the treatment tank 10 and distillate distillate in the recovery tank 40 may be used to remove birch salmon. The active ingredient can be recovered. By adopting the present embodiment, the active ingredient can be extracted almost identically from the birch moss, which has been subjected to cell destruction and cell destruction of birch moss.

  The extracted active ingredients of birch salmon are processed by conventional methods to make functional foods such as confectionery such as caramel, drinks such as juice, powder form and tablet form. Can do. When blended into a functional food, the extract can be blended as it is or as a concentrated extract. Needless to say, a predetermined food additive can be added in the production of the functional food. Thus, by adding the extract containing the active ingredient of the birch salmon of the present invention to the food, there is no off-flavor odor and the like, and it can be made into a functional food that is easy to ingest.

Examples of the present invention will be described below.
(Example 1) Chaga was used as a sample. First, the water in the cell of Chaga was replaced with ethyl alcohol compatible with both liquid carbon dioxide and water in the following manner. The dried chaga was mechanically pulverized and powdered, 10.5 g, was placed in a metal small pressure vessel with an internal volume of 60 ml, and 30 ml of ethyl alcohol was added to seal the vessel. This container was immersed in a hot water bath heated to 40 ° C., liquid carbon dioxide was supplied to the pressure container via a pressure increasing device, pressurized to 15 MPa to be in a supercritical state, and held for 20 minutes. Thereafter, the pressure was slowly reduced to normal pressure. Next, liquid carbon dioxide was again supplied to the pressure vessel via the pressure increasing device, pressurized to 15 MPa and kept in a supercritical state for 20 minutes, and then the pressure was slowly reduced to return to normal pressure. During the two depressurization operations, the carbon dioxide discharged partially contained ethyl alcohol, and 4.01 g was collected in the recovery tank.

  Next, liquid carbon dioxide is supplied to the pressure vessel containing the Chaga processed product via a pressure increasing device, pressurized to 15 Mpa to be in a supercritical state, held for 20 minutes, and then the pressure is released at once. The pressure was quickly returned to normal pressure. Further, liquid carbon dioxide was supplied again via a pressure increasing device, pressurized to 15 MPa, brought into a supercritical state, held for 20 minutes as it was, and then the pressure was released all at once and quickly returned to normal pressure. Thus, a rapid depressurization product of Chaga supercritical carbon dioxide fluid in which intracellular water was replaced with ethyl alcohol was obtained. As a solid, 23.2 g was obtained.

  The weight of dry chaga increased from 10.5 g to 23.2 g by the above treatment. This indicates that a large amount of ethyl alcohol has been taken up into the cell, and the carbon dioxide fluid compatible with ethyl alcohol contained in the cell is converted from a supercritical fluid into a gaseous state. It supports that the cell wall is destroyed by rapid volume expansion.

  Next, 2.07 g of the Chaga-treated product (Chaga in which the cell wall was broken) obtained by the above treatment was placed in a Soxhlet extraction cylindrical filter paper, and Soxhlet extracted overnight using 50 ml of ethyl alcohol as an extraction medium. After completion of the extraction operation, the components remaining on the extraction cylindrical filter paper were dried and weighed to be 0.80 g. Since 2.07 g of the processed chaga product used here corresponds to 0.94 g of the raw chaga, the active ingredient corresponding to 15% of the dried chaga was extracted by this series of treatments. This value was very large compared to the values of Comparative Examples 1 and 2 described later.

  (Comparative Example 1) 1.13 g of a powder sample obtained by mechanically pulverizing dried Chaga was placed in a Soxhlet extraction cylindrical filter paper, and extracted with Soxhlet overnight using 50 ml of ethyl alcohol as an extraction medium. After completion of the extraction operation, the components remaining on the extraction cylindrical filter paper were dried and weighed to be 1.03 g. That is, it was found that the active ingredient corresponding to 9% of the dried chaga was extracted by this treatment.

  (Comparative Example 2) The dried chaga was mechanically pulverized into a powder and further pulverized by a freeze pulverization method using liquid nitrogen to perform cell wall destruction. 1.07 g of this powder sample was put on a Soxhlet extraction cylindrical filter paper, and Soxhlet extraction was performed overnight using 50 ml of ethyl alcohol as an extraction medium. After completion of the extraction operation, the components remaining on the extraction cylindrical filter paper were dried and weighed to be 0.93 g. That is, it was found that the active ingredient corresponding to 13% of the dried chaga was extracted by this treatment.

  As described above, the water contained in the Chaga is once replaced with a medium compatible with the liquid carbon dioxide, which is a supercritical fluid, and then the liquid or supercritical carbon dioxide is allowed to coexist under pressure in the cell wall. It is possible to improve the extraction rate of active ingredients by increasing the carbon dioxide fluid concentration and then destroying the strong cell wall due to the rapid volume expansion accompanying the conversion of carbon dioxide into a gas state by sudden pressure release It was proved.

BRIEF DESCRIPTION OF THE DRAWINGS It is a figure which shows schematic structure of the cell wall destruction apparatus 1 of the birch salmon bamboo as one embodiment of this invention. It is a flowchart which shows the procedure which extracts an active ingredient after crushing the cell wall of a birch bamboo using the cell wall destruction apparatus 1 of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Cell wall destruction apparatus 10 Processing tank 20 Supercritical fluid supply means 21 Liquid carbon dioxide cylinder 22 Supply pump 24 Heat exchanger 31 Gate valve 40 Recovery tank

Claims (5)

Substituting the intracellular water of the birch moth with a medium compatible with both the water and the supercritical fluid;
Replacing at least a portion of the medium in the cell with a supercritical fluid by contacting the birch salmon that has replaced the intracellular water with the medium with a supercritical fluid;
Reducing the pressure at once, and rapidly expanding the supercritical fluid in the cell wall to destroy the cell wall;
A method for destroying a cell wall of a birch tree, which comprises:   The method of claim 1, wherein the supercritical fluid is carbon dioxide, and the medium contains at least one of ethyl alcohol and acetic acid.   A method for extracting an active ingredient of birch moth, which comprises destroying the cell wall of birch moss, and extracting an active ingredient from the birch moth that has destroyed the cell wall by the method for destroying a cell wall of birch moss. Substituting the intracellular water of the birch moth with a medium compatible with both the water and the supercritical fluid;
Replacing at least a portion of the medium in the cell with a supercritical fluid by contacting the birch salmon that has replaced the intracellular water with the medium with a supercritical fluid;
Reducing the pressure at once, and rapidly expanding the supercritical fluid in the cell wall to destroy the cell wall;
Extracting an active ingredient from the birch salmon that has destroyed the cell wall,
A method for extracting an active ingredient of birch moss, wherein the step of destroying the cell wall and the step of extracting the active ingredient from the birch moss that has broken the cell wall are carried out substantially in the same container. A supercritical fluid forming means capable of forming a supercritical fluid;
The birch oyster mushroom, a medium compatible with both water and supercritical fluid, and a treatment tank for destroying the cell wall of birch moth mushroom that can accept the supercritical fluid;
A pressure reducing means capable of reducing the pressure in the treatment tank at once,
A device for destroying the cell wall of Birch fungus, characterized by comprising:

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