JP4977279B2 - Extraction method and apparatus of saponin from ginseng - Google Patents

Description

The present invention relates to an extraction technique for extracting useful substances useful for foods and pharmaceuticals from plant materials. More particularly, selectively supplying the optimum solvent used to extract the saponins from ginseng, by contacting the solvent of optimal conditions for ginseng, efficiently saponins from ginseng extract Related to technology.

  Plants are rich in various useful components having physiologically active functions. As natural compounds, for example, tea contains catechins and is used for health foods. Catechin is a kind of polyphenol, also called tannin, which suppresses active oxygen, which is a cause of body aging and carcinogenic substances. Active oxygen is a substance that changes oxygen in the body, has a strong oxidizing action, and has a bactericidal ability. If it occurs more than necessary, normal cells will be destroyed, and this must be suppressed to some extent.

  Catechin is resistant to bacteria, viruses, etc., has an antihypertensive effect, an antihyperglycemic effect, and a low blood cholesterol lowering effect, and is attracting attention as an effective substance effective for hypertension, diabetes, obesity, arteriosclerosis, etc. . Various extractions of these useful substances have been conventionally proposed. In general, useful substances are extracted using water, hot water, or an aqueous alcohol solution as a raw material, and the extracted substances are concentrated and purified.

  There are many examples of extraction methods from tea. For example, Patent Document 1 describes a method of extracting catechins by irradiating microwaves from tea belonging to the camellia family plant. In addition, a method of extracting water or alcohols as a solvent has been conventionally performed and is known as represented by a method of using hot water. Furthermore, as a method for extracting a physiologically active substance, Patent Document 2 describes a method in which an aqueous solution containing a hydrophobic group-containing water-soluble organic compound and a saccharide and a polar organic solvent are brought into contact with each other.

  On the other hand, as an extraction technique of polyphenols, Patent Documents 3 and 4 show examples of the extraction technique. Patent Document 3 discloses a method of adding ascorbic acid, and Patent Document 4 discloses a method of immersing a plant in water or an alcohol extraction solvent for a predetermined time. Furthermore, as an example of extraction technology, Patent Document 5 describes, as an example of extracting saccharides, contacting cellulose powder with heated hot water heated to a specific temperature, hydrolyzing it, and then rapidly cooling to obtain water-soluble oligosaccharides. Extraction technology, Patent Document 6, discloses a saccharide extraction technology from plant biomass.

  On the other hand, as an example of pigment extraction, Non-Patent Document 1 describes the extraction of anthocyanin pigments from black rice. This document also shows the results of a calibration curve obtained by measuring the absorbance of catechin depending on the extraction solvent, and also shows a comparative example of the extraction efficiency of the polyphenol content.

  Saponin is known as a representative useful substance that can be extracted by applying the present invention. The characteristics of ginseng saponin in the saponin are as follows.

  Saponins are distributed in many plants. Saponins contained in carrots are special saponins that are not found anywhere else. These saponins are known to be both dammaran saponins and oleanol saponins.

1. General effects of saponins Enhancement of immunity, improvement of blood flow, prevention and treatment of blood clots, antidiabetic action, promotion of lipid synthesis and degradation, blood pressure lowering action, stress relieving action, fatigue recovery, etc.
2. Pharmacokinetics and pharmacological action of saponin 1) Activates digestion and absorption function and strengthens non-specific resistance of living body against various stresses. Promotes protein synthesis, enhances metabolism and immunity. There are also tonic and anti-fatigue effects.
2) Effective for anemia caused by various malignant tumors, decreased energy, loss of appetite, cancer pain, etc. Inhibits bone marrow damage, liver damage and immune function decline by invasive treatment, and promotes recovery. It is also effective for improving physical weakness and nutrition due to surgery. Cancer cell growth and metastasis suppression have also been reported.
3) Swelling may occur, and if taken by a fat and ruddy active person (demonstration), in addition to excitement, insomnia, hot flashes, hot flushes, etc., adverse effects such as eczema and increased blood pressure may be seen Because there is, attention is necessary. Do not use if there is an active irritation such as inflammation.

JP 2002-104982 A JP 2003-171328 A JP 2002-97187 A JP-A-7-196645 Japanese Patent No. 3041380 JP 2002-59118 A Gifu City Women's Junior College Bulletin 52nd (March 2003)

  Conventional extraction methods for extracting useful substances from plant materials include decocting in an open kettle or pan (ie, 100 ° C. or less), or batch extraction in a pressure-resistant container such as an autoclave. (For example, Japanese Patent No. 3212278). In contrast, the extraction method of the present invention is an improvement over these conventional extraction methods. Although the extraction methods described in the above-mentioned patent documents are different from each other, extraction is performed using a predetermined solvent in one step. On the other hand, it is known that plants contain a lot of various useful substances.

  The amount of these useful substances to be extracted varies depending on the solvent. Therefore, ideally, it would be sufficient if all useful substances contained in the plant raw material can be extracted, but at present, only the solvent that seems to be optimal for the target plant raw material is contacted for extraction. The plant material is discarded after the extraction. When further extraction is performed, when a new system is used for extraction, useful substances that differ depending on the specific solvent are extracted.

  After extraction with a specific solvent for the same plant raw material in the extraction process of useful substances, if the extraction is changed continuously, such as changing the solvent or changing the temperature in the extraction process, other useful Despite being able to extract the substance, it was disposed of. As described above, plant materials contain a lot of various useful substances. Therefore, if as many useful substances as possible contained in the same plant raw material can be extracted at the same time in a series of extraction processes, the extraction efficiency will be dramatically improved. A technique that can effectively extract useful substances regardless of the type of plant material is further desired.

  The present invention was developed in order to solve such a conventional problem, and achieves the following object.

The object of the present invention is to extract ginseng saponin using a suitable solvent under a wide range of extraction conditions from low temperature normal pressure to high temperature high pressure, and to extract saponin from ginseng, which enables efficient extraction. It is in the provision of the device.

Another object of the present invention is to extract the ginseng saponin by selectively switching the solvent prepared in advance according to the conditions of the plant raw material and supplying it under optimum conditions stepwise or continuously. To provide saponin extraction technology and equipment from ginseng .

  Hereinafter, the present invention takes the following means in order to achieve the object.

The method for extracting saponin from ginseng of the present invention 1 comprises:
A method for extracting saponins from ginseng,
Distilled water, which is a solvent prepared in advance, and a solvent selection step of sequentially selecting one or more of the plurality of solvents from various concentrations of ethanol ;
A solvent supply step of supplying the solvent selected in the solvent selection step;
Heating the selected and supplied solvent to a respective temperature in the temperature range of 100-160 ° C. depending on each solvent ;
An extraction step of contacting the ginseng with the solvent heated in the heating step to extract saponin;
A cooling step of cooling the saponin and the solvent extracted in the extraction step;
A holding step of holding the cooled saponin and the solvent above a certain pressure,
The solvent supplying step is a step of supplying the solvent at a pressure equal to or higher than a saturated vapor pressure at the extraction temperature of the solvent.

Method of extracting saponins from ginseng present invention 2, in the extraction method of extracting saponins from ginseng present invention 1,
The heating step is a step in which the heating temperature of the solvent is heated to 120 ° C.

The method for extracting saponin from ginseng of the present invention 3 is an extraction method for extracting saponin from ginseng of the present invention 1 or 2 ,
The solvent selection step is characterized in that the solvent prepared in advance is distilled water, 70% ethanol, 99% ethanol, and is selected in that order .

Method of extracting saponins from ginseng of the present invention 4, in the extraction method of extracting saponins from ginseng of the present invention 1 to 3, wherein the holding step, holding said solvent in said extraction step on the saturated vapor pressure It is a process to perform.

The method for extracting saponin from ginseng of the present invention 5 is the extraction method for extracting saponin from ginseng of the present invention 1 to 3, wherein the pressure above the saturated vapor pressure of the solvent is 0.1 to 10 MPa. It is characterized by being.

The method for extracting saponin from ginseng of the present invention 6 is the extraction method for extracting saponin from ginseng of the present invention 1 to 3, wherein the extraction time for extracting the saponin is 20 to 60 minutes. It is characterized by.

The method for extracting saponin from ginseng according to the present invention 7 is the extraction method for extracting saponin from ginseng according to the present invention 1 to 3, wherein the predetermined extraction pressure for extracting the saponin is within the temperature range. The pressure range is 0.2 to 2.0 MPa.

The apparatus for extracting saponin from ginseng of the present invention 8 ,
A device for extracting saponins from ginseng,
A solvent storage device for individually storing distilled water as a solvent and ethanol of various concentrations;
A switching device for making a plurality of one or more selections from distilled water and various concentrations of ethanol as the solvent of the solvent storage device;
A high-pressure pump for supplying the solvent supplied via the switching device at a pressure equal to or higher than a saturated vapor pressure in the later-described extraction;
A heating device for heating the solvent supplied by the high-pressure pump to a temperature in a temperature range of 100 to 160 ° C. according to each solvent ;
An extraction device main body for extracting the saponin by contacting the ginseng in a liquid state with the solvent heated and supplied by the heating device;
A cooling device for cooling the extracted saponin;
And a pressure holding device for holding the solvent at a processing temperature at a pressure equal to or higher than the saturated vapor pressure at the processing temperature after the step of supplying the solvent with the high-pressure pump until the end of cooling.

The present invention is constituted by the above means, and more specifically, using a percolator type pressure resistant container, a method of feeding an extraction solvent optimum for the extraction target substance in the plant raw material charged in the container with a high pressure pump Thus, the target substance can be extracted with high yield in a temperature range higher than the boiling point of the solvent and under high pressure conditions. As the solvent, not only water but also an organic solvent, a solvent in which pH and ionic strength are adjusted to the optimum extraction conditions can be used, and the yield of saponin which is a target extraction substance from ginseng can be improved.

Moreover, when extracting saponin from ginseng , it is possible to switch and extract an extraction solvent to distilled water and various concentrations of ethanol by a solvent switching mechanism. The solvent is switched continuously or stepwise. In other words, it is possible to obtain multiple types of extracted substances from the same raw material in a series of flows without using multiple devices, without taking out and charging raw materials multiple times, and without changing the setup. Is possible. By such means, the present invention contributes to simplification of the process, reduction of initial cost, improvement of the yield of the extraction target substance, and the like.

The method for extracting saponin from ginseng of the present invention can be supplied continuously or step by step in a series of processes from a plurality of solvents prepared in advance, regardless of the type. Became. As a result, useful substances such as physiologically active substances can be efficiently extracted under optimum conditions. In addition, many kinds of useful substances can be efficiently extracted by a simple process.

  Hereinafter, specific modes of the present invention will be described as embodiments. This embodiment is mainly applied to plant raw materials (hereinafter referred to as “raw materials”) used for foods and pharmaceuticals, and useful functional substances having physiologically active functions from these raw materials, that is, useful substances (hereinafter referred to as extract substances). , Which is also referred to as an effective substance, but is defined as a synonym in the present invention)). The raw materials are intended to be organic, particularly useful for foods. The target useful substances of the present embodiment are mainly plant extracts such as natural pigments, antibacterial substances, physiologically active substances such as saponins and catechins.

  Catechin and the like are main components of green tea astringency and are a kind of polyphenol. This polyphenol is a general term for plant compounds having a plurality of phenolic hydroxyl groups in the same molecule, and is contained in most plants. It is a substance with excellent antioxidative ability, and is a pigment and bitter component by photosynthesis. Catechin is a representative substance, but this polyphenol is a substance attracting attention for health foods because it is particularly contained in chocolate and cocoa. In addition, saponin is also contained in many plants, but the plant is represented by carrots. This saponin is a useful substance excellent in enhancing immunity. Thus, the present invention is a technique for extracting useful substances from plants such as food.

  The useful substance extraction technique according to the present embodiment will be described with reference to the drawings and tables. FIG. 1 is a diagram showing a concept of a useful substance extraction technique according to the present embodiment, and FIG. 2 is a front view when FIG. 1 is configured as an apparatus having a specific configuration. FIG. 3 is a detailed sectional view of a reactor which is a part of the configuration of this apparatus and extracts a useful substance.

  The reactor 1 is an extraction device main body that forms the center of the configuration of the present invention, in which a raw material 2 that has been crushed or pulverized is inserted, and in the case of the present invention, an organic food material that is a plant. It is intended for. For example, there are ingredients such as tea leaves and ginseng (also called ginseng). The main body of the extractor is charged with these raw materials 2 and is brought into contact with an extraction solvent heated and pressurized to extract useful substances.

  The configuration of the extraction technique relating to the present embodiment includes a solvent tank 3 for individually storing a plurality of different solvents in addition to the main body of the extraction device, and a switching device 5 for selecting and supplying the solvent 4 of these solvent tanks 3. The high-pressure pump 6 that sends out the selected solvent 4 at a high pressure, the heating device 7 that heats the sent solvent 4, and the solvent 4 heated by the heating device 7 is supplied to extract useful substances. The above-described reactor 1, the cooling device 8 for cooling the useful substance extracted in the reactor 1, and the step of supplying the solvent in a high pressure state, that is, the step after the high pressure pump 6 until the end of cooling. And a back pressure valve 9 for maintaining a pressure equal to or higher than the vapor pressure of the solvent at the processing temperature. When it is desired to change the composition ratio of the solvent continuously, a gradient pump may be used.

  Next, a technique for extracting this useful substance will be described in detail with reference to the drawings. As described above, the solvent 4 is supplied to the reactor 1, and this solvent 4 is usually water. In the case of the present embodiment, in addition to water, a plurality of kinds of solvents 4 that are useful and harmless to foods are used, for example, ethanol. These solvents 4 are individually stored in advance in a plurality of solvent tanks 3. The solvents 4 in these solvent tanks 3 are individually stored in advance according to the type of raw material 2 and are most suitable for the extraction reaction. There is no limit to the number of individual solvents 4 to be prepared. As the solvent 4, in addition to water, for example, an organic solvent, alcohol or a mixed solution thereof, a buffer solution, a pH adjusted solution, a solution in which salts are dissolved, or the like that is harmless to the human body is used.

  These solvent tanks 3 are connected to a switching device 5 through pipes or hoses. This switching device 5 is for selecting the solvent 4 of the plurality of solvent tanks 3 by using, for example, a five-way valve, and sending out one or more solvents. The method of selecting and sending out is a case where one solvent is mixed with two or more solvents, one solvent is selected and sent out, and then another solvent is selected and sent out again. By providing this switching device 5, it is possible to widely select the most suitable solvent 4 for extracting useful substances from the raw material 2 according to the extraction object.

  Therefore, by providing this switching device 5, it is possible to select and supply the solvent 4 in the best condition in a stepwise or continuous manner while selecting the solvent 4 in the solvent tank 3 accommodated. The selected solvent 4 is sent to the heating device 7 at a high pressure by the high-pressure pump 6. In the high-pressure pump 6, the solvent 4 is pressurized at least higher than the vapor pressure indicated by the solvent at the time of heating, and the inside of the apparatus is kept in a liquid phase (pressurized hot water). At this time, the highest possible pressure can improve the extraction efficiency. When extracting catechins from tea leaves, it is effective to set to 10.1 MPa (100 atm). In the range where the extraction effect does not decrease even at low pressure, it may be 10.1 MPa (100 atm) or less, for example, 1.0 Mpa (10 atm).

  However, in the case of less than that, in the extraction of catechin, the extraction temperature is from room temperature to 80 ° C. and from 80 ° C. to 140 ° C., which is a two-stage setting temperature for performing extraction twice. For example, in order to maintain a liquid phase at a temperature of 130 ° C. using water, for example, the pressure needs to be 0.27 MPa (2.65 atm) or more. More specifically, the extraction of catechin is preferably performed by raising the temperature to 120 ° C. In the case of water at 120 ° C. or higher, the pressure is 0.2 MPa or higher, but considering the non-uniform temperature distribution of the apparatus, 0.4 MPa or higher is preferable, and in consideration of safety, pressure up to 1 MPa is required. An extraction pressure of 0.4 MPa or more is required at 140 ° C., but a pressure of up to 1 MPa can be sufficiently covered. On the other hand, since chlorophyll extraction is preferably performed at 90 ° C. or lower, catechin is first extracted with ethanol at about 90 ° C. and then heated to 80 ° C. or higher, preferably 120 ° C. or higher as described above. The kind is extracted.

  For saponins, the extraction yield is low at 100 ° C. or lower, and extraction in the temperature range of 100 to 160 ° C. is preferred. The extraction pressure corresponding to the above-mentioned temperature range at this time is preferably a pressure range of 0.2 to 2.0 MPa. More specifically, when the temperature is 100 ° C. or higher, the extraction pressure is 0.2 MPa or more. When the temperature is 120 ° C. or more, the extraction pressure is 0.4 MPa or more. When the temperature is 160 ° C., the extraction pressure is 1.2 MPa or more. However, in consideration of safety, it is preferable to set the extraction pressure up to 2.0 MPa. In order to detect this pressure, a pressure sensor 10 is provided in the supply process.

  Further, for the sake of safety, a relief valve 11 is similarly provided for releasing the solvent to the outside and keeping the pressure constant when the pressure becomes abnormally high. Further, the supplied solvent is guided to the heating device 7 via the three-way valve 12, and excess solvent is recovered outside the system via the drain 13 in the course of this route. The set value of the pressure of the high-pressure pump 6 is determined by a practical numerical value in consideration of the extraction efficiency of the extraction target substance, the pressure resistance of the extraction device, the pressurization capacity of the pump, and the like.

  The solvent 4 is increased in pressure in this way and guided to the heating device 7 to be heated. The heating device 7 includes a heating serpentine tube 14, and the heating serpentine tube 14 is immersed in a heated oil tank 15 or a salt bath, and the solvent 4 is heated by heat exchange when passing through the heating serpentine tube 14. Is done. However, the heating device 7 is not limited to this configuration. The solvent 4 is hydrothermalized in the case of water, for example, when the raw material is tea leaves, the temperature is from room temperature to 120 ° C., more preferably from room temperature to 80 ° C. and from 80 ° C. to 120 ° C. in steps. It is good to extract by setting the temperature.

  The temperature at this time is the most suitable temperature for extracting useful substances, but a temperature up to 140 ° C. is suitable for extraction. The reason for pressurizing and hydrothermalizing in this way is to improve the yield of extraction of useful substances from the raw material 2. Since this heating temperature varies depending on the type of the raw material 2, the heating temperature is set so as to be optimal for the raw material 2. When the solvent 4 is supplied to the reactor 1, the temperature is controlled by a temperature sensor 16 such as a thermocouple.

  By this temperature control, the solvent 4 can be set to various temperatures in accordance with the raw material 2 and can be always kept at a constant temperature. In this way, the extraction temperature can be controlled. The lower limit is equal to or higher than the freezing point of the solvent 4, but if the pressure resistance of the entire apparatus is increased, the high temperature side can be set even at a temperature higher than the critical point. Pressurized hot water in the range of this condition is supplied to the reactor 1 through a pipe, and brought into contact with the raw material 2 charged in the reactor 1 to extract useful substances. The reactor 1 is for extracting useful substances. The reactor 1 has a shape as shown in FIG. 3 and is a cylindrical body made of stainless steel and having a hollow inside.

  Stainless steel porous filters 1 a are detachably fixed to the upper and lower ends of the reactor 1. This porous filter 1a has a through hole in the range of 2 to 100 μm. The material of the porous filter 1a is not limited to stainless steel but may be porous ceramic. What is necessary is just to select and fix the most suitable hole in consideration of the particle size of the raw material. At the upper and lower ends of the reactor 1, a supply port 1b for supplying the solvent 4 and a discharge port 1c for the extracted useful substance are provided. The raw material 2 charged in the reactor 1 is chopped or powdered and is easily extracted. Preferably, the pulverized particles are about 12 mesh, but tea leaves and the like need not be pulverized.

  Since the raw material 2 is sandwiched between the porous filters 1a, it does not flow out of the reactor 1. A heating jacket 1d is incorporated in the outer periphery of the reactor 1 to hold the extraction solvent heated under pressure at a constant temperature. The heating jacket 1d is a heat exchanger for heating the reactor 1 from the outside with a heat transfer heater or heat medium oil. The extraction time in this reactor 1 is usually in the range of 5 to 240 minutes. When limited to the extraction of saponin from ginseng or catechin from tea in the examples, the range of 20 to 60 minutes is preferable. This time range is the most suitable temperature range in which extraction is possible, but in practice, the optimal time is specified and set according to the type of raw material 2 and extraction conditions.

  In the setting of the extraction process, for example, after the extraction is performed in the first process set at a predetermined temperature, the extraction can be performed in the second process set at a different predetermined temperature. At this time, changing the extraction time or changing the type of solvent is accompanied. For example, when the raw material 2 is tea leaves, the temperature is set in the range from room temperature to 80 ° C. in the first step and then extracted, and then the temperature is set in the range from 80 ° C. to 120 ° C. in the second step. Perform extraction. Furthermore, the solvent is switched from water to ethanol during the extraction process and vice versa. Alternatively, the third extraction can be performed as a third step by changing the solvent after the second extraction.

  The useful substance discharged from the reactor 1 is cooled as a solution or a suspension by the cooling device 8 to a temperature equal to or lower than the boiling temperature of the solvent under atmospheric pressure (usually room temperature level). This cooling is for suppressing thermal decomposition and thermal denaturation of useful substances and preventing boiling of the solvent flowing out. The cooled useful substance passes through the three-way valve 12 and is finally discharged to the outside through the back pressure valve 9 and stored in the recovery tank 17 or the like. This back pressure valve 9 keeps the pressure of the solvent 4 higher than the vapor pressure of the solvent 4 at the processing temperature during the process of supplying the solvent 4 in a high pressure state, that is, the process after the high pressure pump 6 until the end of cooling. In order to keep the inside of the apparatus in a liquid phase. A pressure gauge 18 is provided to detect this pressure holding state, and the pressure is checked. By maintaining the pressure, an extraction operation in a temperature region above the boiling point of the solvent 4 becomes possible. Further, this apparatus is provided with a control device 19 and switches for electrically controlling a temperature controller, a pressure controller and the like in the series of flows. The three-way valve 12 also functions as backwashing when the filter is clogged.

  As mentioned above, although embodiment of this invention was described, it cannot be overemphasized that this invention is not limited to this. Although the present embodiment has been described mainly with respect to extraction of food-related useful substances such as saponins and catechins, extraction of natural pigments and the like may be used. Although details are not described, extraction can be performed by the same method as described above. The examples described later are examples in the case where the solvent is water and ethanol and a useful food-related substance is extracted, but the type is not limited as long as it is a solvent useful for extraction. A solvent most suitable for the conditions of the raw material may be applied. The extraction technology for useful substances has been described above, but after completion of extraction, the temperature conditions are increased under the condition that the solvent is water, and the hemicellulose, cellulose, and lignin in the plant body are hydrolyzed to dissolve water-soluble sugars and easily suspended. It goes without saying that the process can be continuously performed to obtain a sex lignin.

  Hereinafter, specific experimental examples will be described as examples. Examples using water and ethanol as the solvent are shown in FIGS. In this example, tea leaves are applied as a raw material and the extraction behavior of 1 g of tea leaves is shown. The yield for each process under different conditions is shown. FIG. 4 shows an example in which ethanol is used as a solvent and then changed to water. FIG. 5 shows an example in which the solvent is changed to ethanol after use as water. Each time was changed for each process, and the amounts of extracted useful substances, that is, catechin and chlorophyll were compared as yields.

  In FIG. 4, the amount of extraction is the largest in the case of step 2, and the amount of extraction is confirmed in other steps as well. The amount of residue is 20-30%. In FIG. 5, in the case of the process 1 (80 degrees C or less water), the amount of extraction is the largest, and it can confirm that it extracted in a short time compared with FIG. The amount of residue is 30-40%. It shows that the best extraction conditions can be set by changing the solvent selection conditions.

  Table 1 shown below shows the results of the catechin extraction amount extracted for each type of catechin by changing the temperature condition of the solvent in the example where the raw material is tea leaves. An example in which the solvent was extracted as water and then replaced with ethanol was shown. Table 2 is an example in which the raw material is tea leaves, and shows a comparison of the amount of catechin extracted between the case of the present invention and the conventional case.

  The example of Table 1 is based on the example of FIG. 5 and shows catechins numerically for each type. The result of extracting by changing the temperature setting step by step is shown. That is, catechin extraction was performed on tea leaves at room temperature to 80 ° C. as the first step, and catechin extraction was performed again on the tea leaves at a temperature range of 80 ° C. to 120 ° C. after the extraction. After this second step, the solvent was switched from water to ethanol at a temperature of 120 ° C., and chlorophyll was extracted as the third step.

  As a result, different results were obtained depending on the type of catechin. Among the many types of useful substances, some were not extracted even when the solvent was switched to ethanol, but the types of catechins described were extracted in different stages, but the extraction results were comprehensive. The catechin yield is improved. It was confirmed that extraction by solvent switching and process switching was effective.

The examples in Table 2 show the results of extraction using an open container at a set temperature within 80 ° C. at normal pressure, that is, the method according to the present invention, that is, the heating temperature is stepped up to 120 ° C. It shows a comparison with the results of Table 1 extracted in a higher manner. The result of the present example shows the total amount of catechin extracted in the first step and the second step of Table 1 described above. The solvent is only water. Depending on the type of catechin, there are some that do not have an extraction effect when viewed individually, but in the case of this example, the total amount of catechin extraction is about 40% higher than the conventional yield. The usefulness of this example was confirmed.

  FIG. 6 shows the visible region spectra of the ethanol extract and the hot water extract at 120 ° C. (omitted because the spectrum of the water extract at a temperature of 120 ° C. or lower was also of substantially the same absorption). . In the extraction experiment, after extraction with hot water at 120 ° C., extraction was performed by switching the solvent to 99% ethanol at the same temperature, and obtaining a visible region spectrum of the extract. As shown in FIG. 6, catechins were almost entirely extracted by hot water extraction up to 120 ° C., and almost no contamination was found in the ethanol extraction fraction. Instead, chlorophyll, a fat-soluble substance, is selectively dissolved in the ethanol extraction fraction.

Chlorophyll is a substance having absorption at 350 to 450 nm and 650 to 700 nm, and has high utility value as a natural pigment. The ethanol extract contained a large amount of chlorophyll, and its absorption was observed at around 660 nm as shown in the figure. Therefore, by the pressurized solvent extraction method, first, catechins were extracted at a high yield while raising the temperature to 120 ° C. using water as the solvent, and then a large amount of impurities-free chlorophyll was obtained by switching the extraction solvent to ethanol. It was confirmed that extraction was possible.
In addition, the abbreviation symbol of catechin shown in the figure is catechin shown below.
G: Garlic acid EC: Epicatechin EGCG: Epigallocatechin gallate ECG: Epicatechin gallate EGC: Epigallocatechin

  Next, saponin extraction data according to another example in which the plant as a raw material is ginseng (ginseng) is shown in FIGS. In the case of Example 4, the amount of increase in extraction is shown in total. The total extraction yield was confirmed. In this example (circulation formula), the yield of saponin according to each extraction temperature was confirmed for each amphiphilic property. Ginseng used white ginseng and was 12-42 mesh (380-1680 μm).

  There were three solvents: distilled water, 70% ethanol, and 99% ethanol. As an implementation condition, each effluent was collected under the temperature conditions of 100 ° C., 120 ° C., and 160 ° C. at a liquid flow rate of 3 ml / min. The time required for the temperature increase was 20 minutes for each temperature increase. After the temperature rise, the effluent (180 ml) was collected by holding for 40 minutes, lyophilized and analyzed for saponin by HPLC. The pressure was adjusted with a back pressure valve to 2 MPa.

  Furthermore, a method (batch type) different from the method of the present invention was performed for comparison. As described above, distilled water, 70% ethanol, and 99% ethanol were used as the extraction solvent. In this batch method, 1.0 g of crushed carrot was placed in a beaker and extracted with 100 ml of solvent for 1 hour. After decantation of the extraction solvent, 100 ml of fresh solvent was newly added, extraction was performed for 1 hour in the same manner, the same operation was repeated, and extraction with 300 ml of solvent was performed. As before, the saponin was analyzed by HPLC after freeze-drying the extract.

  Ginseng saponins were classified into hydrophilic, amphiphilic (water and oil), and lipophilic depending on the amphiphilic properties. The figure is a data diagram showing the total as a batch system and the yield for each temperature of 100 ° C, 120 ° C, and 160 ° C. FIG. 7 shows the case where the solvent is distilled water, FIG. 8 shows the case where the solvent is 70% ethanol, and FIG. 9 shows the case where 99% ethanol. As a result of this data, the yield of saponin is higher in the flow method of the present invention than in the batch method for each solvent.

  According to the data, the yield tends to be slightly improved when the temperature is partially 70% ethanol, but when considering other cases, the optimum extraction is generally at 120 ° C. And the yield is improved. FIG. 10 collectively shows the case at 120 ° C. As a result, the tendency of yield at the same temperature is extracted in the case of distilled water in which a lot of hydrophilic substances are extracted, in the case of 70% ethanol, a lot of amphiphilic substances are extracted, and in the case of 99% ethanol, it is lipophilic. Many things have been extracted. As a result, the following was confirmed.

  In the extraction at 120 ° C., for example, when the extraction solvent is sequentially switched in the order of distilled water → 70% ethanol → 99% ethanol, the extraction is performed for most of water-soluble (hydrophilic) to fat-soluble (lipophilic). Saponin can be extracted simultaneously. In addition, it was also confirmed from this example that saponin can be extracted effectively by performing extraction while switching the temperature to the optimum temperature for each solvent.

FIG. 1 is a conceptual diagram showing an extraction process for extracting useful substances. FIG. 2 is a block diagram of an apparatus for extracting useful substances. FIG. 3 is a cross-sectional view of the reactor. FIG. 4 is a data diagram showing comparative data of yields of useful substances by changing the solvent conditions in an example in which the plant of the raw material is tea leaves. The Example which changed the solvent from ethanol to water is shown. FIG. 5 is a data diagram showing comparative data on yields of useful substances by changing the solvent conditions in an example where the raw material plant is tea leaves. The Example which changed the solvent from water to ethanol is shown. FIG. 6 is a view showing a visible absorption spectrum of a solution containing an extraction substance. The peak around 660 nm indicates absorption of chlorophyll. FIG. 7 is a data diagram showing the yield of saponin (per 1 g of dried carrots) in which the raw material plant is another example of ginseng, using distilled water as a solvent and adding lyophilicity at each temperature. FIG. 8 is a data diagram showing the yield of saponin (per 1 g of dried ginseng) in which the raw material plant is another example of ginseng, the solvent is 70% ethanol, and the amphiphilic properties are taken into account at each temperature. FIG. 9 is a data diagram showing the yield of saponin (per 1 g of dried ginseng) in which the raw material plant is another example of ginseng, the solvent is 99% ethanol, and lyophilicity is added at each temperature. FIG. 10 is a data diagram showing the saponin yield (per 1 g of dried ginseng) of each solvent at 120 ° C., where the plant as a raw material is another example of ginseng.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... Reactor 2 ... Raw material 3 ... Solvent tank 4 ... Solvent 5 ... Switching device 6 ... High pressure pump 7 ... Heating device 8 ... Cooling device 9 ... Back pressure valve

Claims (8)

A method for extracting saponins from ginseng,
Distilled water, which is a solvent prepared in advance, and a solvent selection step of sequentially selecting one or more of the plurality of solvents from various concentrations of ethanol ;
A solvent supply step of supplying the solvent selected in the solvent selection step;
Heating the selected and supplied solvent to a respective temperature in the temperature range of 100-160 ° C. depending on each solvent ;
An extraction step of contacting the ginseng with the solvent heated in the heating step to extract saponin;
A cooling step of cooling the saponin and the solvent extracted in the extraction step;
A holding step of holding the cooled saponin and the solvent above a certain pressure,
The method for extracting saponins from ginseng, wherein the solvent supplying step is a step of supplying the solvent at a pressure equal to or higher than a saturated vapor pressure at the extraction temperature of the solvent. In the extraction method which extracts the saponin from the ginseng of Claim 1,
The method for extracting saponin from ginseng, wherein the heating step is a step of heating the solvent to 120 ° C. In the extraction method which extracts the saponin from the ginseng of Claim 1 or 2,
In the method for extracting saponins from ginseng, the solvent selection step includes distilled water, 70% ethanol, and 99% ethanol prepared in advance. In the extraction method of extracting saponins from ginseng according to item 1 which is selected from claims 1 to 3,
The method for extracting saponin from ginseng, wherein the holding step is a step of holding the solvent in the extraction step at a saturated vapor pressure or higher. In the extraction method which extracts the saponin from the ginseng of Claim 1 selected from Claim 1 thru | or 3,
The method for extracting saponins from ginseng, wherein the pressure above the saturated vapor pressure of the solvent is 0.1 to 10 MPa. In the extraction method which extracts the saponin from the ginseng of Claim 1 selected from Claim 1 thru | or 3,
The method for extracting saponins from ginseng, wherein an extraction time for extracting the saponins is 20 to 60 minutes. In the extraction method which extracts the saponin from the ginseng of Claim 1 selected from Claim 1 thru | or 3,
The method for extracting saponin from ginseng, wherein a predetermined extraction pressure for extracting the saponin is a pressure range of 0.2 to 2.0 MPa with respect to the temperature range. A device for extracting saponins from ginseng,
A solvent storage device for individually storing distilled water as a solvent and ethanol of various concentrations;
A switching device for making a plurality of one or more selections from distilled water and various concentrations of ethanol as the solvent of the solvent storage device;
A high-pressure pump for supplying the solvent supplied via the switching device at a pressure equal to or higher than a saturated vapor pressure in the later-described extraction;
A heating device for heating the solvent supplied by the high-pressure pump to a temperature in a temperature range of 100 to 160 ° C. according to each solvent ;
An extraction device main body for extracting the saponin by contacting the ginseng in a liquid state with the solvent heated and supplied by the heating device;
A cooling device for cooling the extracted saponin;
From the step of supplying the solvent with the high-pressure pump to the end of cooling, a saponin from Panax ginseng comprising a pressure-holding device for maintaining a pressure equal to or higher than the saturated vapor pressure of the solvent at the processing temperature. Extraction device.

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