JP3559994B2 - Extraction method of mushroom components - Google Patents

Description

Some mushrooms have been prized as a herbal medicine since ancient times, some are loved by gourmets, and others are on the daily table. Various. The nutritional characteristics that can be said about mushrooms in general are that they have low sodium and high potassium, and it is well known that this potassium has a function of lowering blood pressure. In addition, it is a calorie-free food without fear of cholesterol accumulation, and contains various digestive enzymes such as amylase, and many vitamins B ₁ and B _{2 which} are essential for metabolism.

  Apart from matsutake, shimeji, enokitake, shiitake and mushrooms, new mushrooms have appeared on the market in recent years. In addition, as a Chinese medicine, Bukuryo and Chorei have been used for a long time, and have been used for the purpose of irrigation and anticancer effects. Agaricus, reishi and shiitake mushrooms are used as health foods, and their effects have been recognized clinically. Lentinan of Shiitake mushroom, Krestin of Kawatake mushroom, Schizophyllan of Suehirotake mushroom and the like are used for medical treatment as anticancer agents, and the anticancer activity of β-glucan which is a polysaccharide in agaricus has been attracting attention.

Conventionally, various methods for extracting mushrooms have been considered, but extraction with hot water is common. However, the high-molecular-weight fraction, for example, β-glucan, cannot be completely extracted by the hot water extraction, and remains in the extracted substance. By hot-water alkali extraction, β-glucan and the like in the high molecular fraction can be extracted in a considerable amount, but there is a drawback that when extracted, the alkali concentration becomes high. When neutralized, it is considered that the salt concentration becomes high and the salty taste becomes strong. In addition, a high molecular fraction, β-glucan, etc., is also taken out by enzymatic decomposition.However, only the improvement of the β-glucan recovery efficiency is considered, and substances considered to be pharmacologically useful are also lost by the enzyme. It is possible that
However, these methods merely consider a means for producing an extract, or simply to efficiently extract a high molecular fraction, and extract all useful components contained in mushrooms. It is considered that it is hard to say that there is.

  It is an object of the present invention to provide a method for simply obtaining an extract extract or a method for efficiently obtaining a β-glucan of a high molecular fraction, as in the conventional extraction method, but not a low molecular fraction of mushrooms. By extracting the intermediate fraction and the high molecular fraction individually or in a mixed state, the useful components contained in the mushrooms can be thoroughly extracted, and the useful components can also be extracted from the extracted cake. It is to provide a method that can be performed.

The present invention has been made to solve the above problems,
(I) A method for extracting mushroom components, comprising the following steps (1) to (6).
(1) a step of extracting raw, frozen or dried mushrooms in 5 to 100 parts by weight of water at 30 ° C. or lower per 1 part by weight of the mushrooms;
(2) The raw, frozen or dried mushrooms and the extraction residue in the step (1) , or the extraction residue in the step (1) are treated with 5 to 5 parts by weight of the mushrooms and / or the extraction residue. Extracting in 100 parts by weight of water at 70 ° C. or higher,
(3) converting the raw, frozen or dried mushrooms and the extraction residue in the step (1) and / or (2) or the extraction residue in the step (1) and / or (2) into the mushrooms and / or Extracting by subjecting the extract residue to enzymatic treatment with a plant tissue degrading enzyme derived from a filamentous fungus in water at 30 to 90 ° C. in an amount of 5 to 100 parts by weight based on 1 part by weight of the extraction residue;
(4) a step of separately separating the fractions obtained in steps (1) to (3) by solid-liquid separation by centrifugation and / or filtration;
(5) a step of separately concentrating the obtained clear separated liquid; and (6) a step of separately drying the obtained concentrated liquid;
Is provided.
Also, the present invention
(II) The method according to (I), wherein the plant tissue-disintegrating enzymes derived from filamentous fungi are cellulase and pectinase.
( III ) The method according to (I) or (II) , wherein in step (1), the mixture is extracted by mixing with a stirrer.
( IV ) The method according to (I) or (II) , wherein in step (1), the mushrooms are immersed in water, sufficiently contacted with water, and allowed to stand naturally for extraction without mixing with a stirrer,
( V ) In step (1), stirring or leaving naturally in 5 to 100 parts by weight of 30 to 100% ethanol instead of 5 to 100 parts by weight of water. The method according to (I) or (II) , wherein
( VI ) The method according to (I) or (II) , wherein in step (1), the surface of the mushrooms is washed away with running water, and the water is collected and extracted.
( VII ) In Steps (1) to (3), Steps (2) and (3) are performed without adding fresh, frozen or dried mushrooms to Steps (1) to (2) and (3). By repeating the extraction sequential steps, the low-molecular fraction from step (1), the low-molecular and high-molecular fraction from step (2), and the high-molecular fraction from step (3) are separated separately. A method according to (I) or (II) ,
( VIII ) The method according to (I) or (II) , wherein in step (4), filtration is performed after centrifugation.
( IX ) The method according to (I) or (II) , wherein in the solid-liquid separation by filtration in step (4), a filter aid selected from the group consisting of diatomaceous earth, celite, perlite, and crystalline cellulose is used.
( X ) The method according to (I) or (II) , wherein in step (2) and (3), the residue of mushrooms separated is dried and powdered.

  The extract obtained by the method of the present invention is an extract that can be widely used in the fields of seasonings, health supplements, food raw materials and the like. In addition, the final residue from which the high molecular fraction has been taken out can be usefully used as a water-insoluble dietary fiber by drying and pulverizing, and the resources of mushrooms can be used without waste.

  The present invention is a method in which useful components contained in mushrooms can be used without waste by extracting the components of the mushrooms in units of molecular weight. It has utility value for each use, and it can be used in a wide range of applications including seasonings, health foods, food ingredients, immunoactive foods containing a large amount of high-molecular polysaccharides represented by β-glucan, and natural dietary fiber derived from mushrooms. The present invention provides extracts that can be easily processed into preparations, tablets, granules and the like.

Hereinafter, the present invention will be described in detail.
The mushrooms used in the extraction method of the present invention may be from any place of origin, fresh, frozen, dried, etc., but those which are free from microbial contamination, high concentration of pesticide residues, and little foreign matter are desirable.
First, in step (1), fresh, frozen or dried mushrooms are mixed with 5 to 100 parts by weight of cold water at 30 ° C. or lower per 1 part by weight of mushrooms, or 5 to 100 parts by weight of 30 to 100 ° C. or lower at 30 ° C. or lower. It is poured into an aqueous ethanol solution of 10% and extracted.
Extraction is performed by mixing the mushrooms in a stirrer, or without mixing with a stirrer, immersing the mushrooms in water and bringing them into sufficient contact with water, leaving them to stand naturally, or washing the surface of the mushrooms with running water, Is carried out by collecting
The extraction time is adjusted depending on the amount of cold water or ethanol aqueous solution. The Brix solid content concentration is checked at appropriate intervals, and the time when the value no longer changes is regarded as the end time. In the step (1), mainly low-molecular components are extracted from the components contained in the mushrooms.

  In the step (4), the thus extracted liquid is subjected to solid-liquid separation of a water-insoluble portion by a centrifuge. When the centrifugal force is high, the separated solution can be used as it is, but when the centrifugal force is low, by performing microfiltration using a filtration device such as a filter cylinder or a filter press, it is clearer than the liquid using only a centrifuge. Liquid can be obtained. Although a filtration device alone is possible, a device having a large filtration area is required. Further, by using diatomaceous earth, celite, perlite, crystalline cellulose, etc. as a filter aid in an amount of 5 to 150% by weight based on the weight of the mushrooms, water-insoluble lipids in the mushrooms can be adsorbed and removed. Can be. Further, a clearer liquid can be obtained by using a filter aid.

The liquid thus obtained is concentrated under reduced pressure at 60 ° C. or lower in a step (5) using a concentrator. The amount of the concentrated liquid is adjusted to an appropriate weight depending on the conditions of use and storage.
The concentrated solution obtained in this way is sterilized by heat and then refrigerated, frozen or stored, or sterilized by heat or afterward, suitable acid, preferably hydrochloric acid, apple, which is recognized as an additive for food additives. By adding acid, citric acid, tartaric acid, lactic acid, acetic acid, fumaric acid, phthalic acid, gluconic acid, adipic acid, vinegar, etc., the pH is generally adjusted to 4.2 or less, preferably to 3.9 or less. Propagation of the microorganisms can be suppressed.

The concentrated solution thus obtained can be used as it is, but can be dried and powdered by a freeze dryer, a spray dryer or the like in step (6).
Next, in the step (2), the residue of the mushrooms obtained by the extraction in the step (1) is put into 5 to 100 parts by weight of hot water at 70 ° C. or more based on 1 part by weight of the residue. Is extracted with stirring for 30 to 300 minutes.
The heating time needs to be shorter when the temperature is higher, and longer when the temperature is lower. For example, preferably, the temperature is preferably 70 ° C. for 2 to 5 hours and 95 ° C. for 30 to 180 minutes.
In step (2), raw, frozen or dried mushrooms can be extracted instead of or together with the extraction residue in step (1).
When extracting fresh, frozen or dried mushrooms in place of the extraction residue in step (1), the extraction is performed in 5 to 100 parts by weight of water with respect to 1 part by weight of the mushrooms. When the mushrooms and the extraction residue of step (1) are to be extracted together, they are extracted in 5 to 100 parts by weight of water based on 1 part by weight of the total.
When only the extraction residue in step (1) is extracted, a component intermediate between a low molecular weight and a high molecular weight mainly from the components contained in the mushrooms is extracted. When only mushrooms are extracted, mainly low molecular components and intermediate components are extracted. When extracting both mushrooms and the extraction residue of step (1), mainly low molecular components and intermediate components are extracted.

In the step (4), the liquid thus extracted is subjected to solid-liquid separation of a water-insoluble portion by a centrifuge. When the centrifugal force is high, the separated solution can be used as it is, but when the centrifugal force is low, by performing microfiltration using a filtration device such as a filter cylinder or a filter press, it is clearer than the liquid using only a centrifuge. Liquid can be obtained. Although a filtration device alone is possible, a device having a large filtration area is required. Further, by using diatomaceous earth, celite, perlite, crystalline cellulose, etc. as a filter aid in an amount of 5 to 150% by weight based on the weight of the mushrooms, water-insoluble lipids in the mushrooms can be adsorbed and removed. Can be. Further, a clearer liquid can be obtained by using a filter aid.
The liquid thus obtained is concentrated under reduced pressure at 60 ° C. or lower in a step (5) using a concentrator. The amount of the concentrated liquid is adjusted to an appropriate weight according to the conditions of use and storage.

The concentrated solution obtained in this way, by refrigeration or frozen storage after heat sterilization, or during heat sterilization or after heat sterilization, an appropriate acid, preferably hydrochloric acid, malic acid, which is recognized as a food additive, By adding citric acid, tartaric acid, lactic acid, acetic acid, fumaric acid, phthalic acid, gluconic acid, adipic acid, vinegar and the like, the pH is adjusted to 4.2 or less, preferably to 3.9 or less. The proliferation of microorganisms can be suppressed.
The thus obtained concentrated liquid can be used as it is, but can be dried and powdered by a freeze dryer, a spray dry dryer or the like in the step (6).

Next, in the step (3), the residue of the mushrooms obtained by the extraction in the step (1) and / or (2) is heated at 30 to 90 ° C. in an amount of 5 to 100 parts by weight based on 1 part by weight of the residue. Pour into water and warm water and stir and mix. Next, 0.001 to 5.0% by weight of the fungus-derived plant tissue-disintegrating enzyme is added to 1 part by weight of the mushroom residue and mixed with a stirrer or the like. The preferred temperature is 40 to 60 ° C, and the enzyme treatment time is suitably 2 to 12 hours.
In step (3), raw, frozen or dried mushrooms can be extracted instead of or together with the extraction residue of step (1) and / or (2).
When extracting raw, frozen or dried mushrooms in place of the extraction residue in step (1) and / or (2), the extraction is performed in 5 to 100 parts by weight of water per 1 part by weight of the mushrooms. When the mushrooms and the extraction residue of step (1) and / or (2) are to be extracted together, extraction is carried out in 5 to 100 parts by weight of water with respect to 1 part by weight of the total.
When extracting only the extraction residue of step (1) and / or (2), mainly high molecular components are extracted from the components contained in the mushrooms. When only mushrooms are extracted, low molecular components are extracted. When extracting both mushrooms and the extraction residue of step (1) and / or (2), low molecular components or high molecular components are extracted.

The enzyme reaction treatment time and treatment temperature may vary slightly depending on the type, amount, maker, titer, or combination of two or more types of enzymes, so that adjustment is considered necessary.
The enzyme-treated extract is heat-treated at 70 ° C. or higher for 10 to 120 minutes to inactivate the enzyme to obtain a final extract.

  The water-insoluble portion of the extract thus obtained is subjected to solid-liquid separation in a step (4) by a centrifuge. When the centrifugal force is high, the separated solution can be used as it is, but when the centrifugal force is low, by performing microfiltration using a filtration device such as a filter cylinder or a filter press, it is clearer than the liquid using only a centrifuge. Liquid can be obtained. Although a filtration device alone is possible, a device having a large filtration area is required. Further, by using diatomaceous earth, celite, perlite, crystalline cellulose, etc. as a filter aid in an amount of 5 to 150% by weight based on the weight of the mushrooms, water-insoluble lipids in the mushrooms can be adsorbed and removed. Can be. Further, a clearer liquid can be obtained by using a filter aid.

  The liquid thus obtained is concentrated under reduced pressure at 60 ° C. or lower in a step (5) using a concentrator. The amount of the concentrated liquid is adjusted to an appropriate weight depending on the conditions of use and storage.

  The concentrated solution obtained in this way, by refrigeration or frozen storage after heat sterilization, or during heat sterilization or after heat sterilization, an appropriate acid, preferably hydrochloric acid, malic acid, which is recognized as a food additive, By adding citric acid, tartaric acid, lactic acid, acetic acid, fumaric acid, phthalic acid, gluconic acid, adipic acid, vinegar and the like, the pH is adjusted to 4.2 or less, preferably to 3.9 or less. The proliferation of microorganisms can be suppressed.

The concentrate thus obtained can be used as it is, but can be dried and powdered by a freeze dryer, a spray dryer or the like in step (6).
The extraction residue obtained from the step (2) or (3) finally obtained is dried at 40 ° C. or more using a tray dryer, a flow dryer or the like. The dried extraction residue is pulverized to a suitable size, and a fine powder is obtained using a pulverizing powder machine such as a mortar or a ball mill.
Although it has been described above that the separated liquids from the extraction steps (1) to (3) are separately separated into solid and liquid, concentrated and dried, these separated liquids may be arbitrarily combined, for example, all may be put together. , The solid-liquid separation and concentration can be performed continuously to obtain a concentrated solution containing low to high molecules.

  Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited thereto.

100 kg of dried Hanabitake mushrooms is put into 1,500 kg of cold water at 20 ° C., and extracted with stirring for 2 hours.
Next, the residue is subjected to solid-liquid separation by an effective wall centrifuge.
The liquid subjected to solid-liquid separation is rotated at 13,000 to 15,000 in a Sharpless centrifuge to pass the liquid, and further subjected to solid-liquid separation. The separated liquid is passed through a stainless steel filter to which 5 kg of diatomaceous earth is attached to obtain a clear liquid.
The filtered liquid is concentrated under reduced pressure at a temperature of 60 ° C. or lower to make the final liquid volume 40 kg. The container is sterilized by heating at 90 ° C. for 30 minutes and filled in a hot state.
The obtained concentrate was a solution containing a large amount of low molecular fraction containing about 20 to 60% of sugar alcohol such as mannitol and sorbite.

100 kg (at the time of drying) of the dried extract of Hanabitake mushroom in Example 1 is poured into 1,500 kg of hot water at 90 to 100 ° C, and the mixture is stirred and extracted for 2 hours.
Next, the residue is subjected to solid-liquid separation by an effective wall centrifuge.
The liquid subjected to solid-liquid separation is rotated at 13,000 to 15,000 in a shear press type centrifuge to pass the liquid, and further subjected to solid-liquid separation. The separated liquid is passed through a stainless steel filter to which 5 kg of diatomaceous earth is attached to obtain a clear liquid.
The filtered liquid is concentrated under reduced pressure at a temperature of 60 ° C. or lower to make the final liquid volume 30 kg. The container is sterilized by heating at 90 ° C. for 30 minutes and filled in a hot state.
The resulting concentrated solution was able to extract 5% or less of sugar alcohols such as mannitol and sorbit, and about 5 to 20% of the total content of dried water-soluble polysaccharides including β-glucan and the like in the dried mushroom mushroom. Solution.
Dextrin in the same amount as the solid content was added to the obtained concentrated liquid, and dried with a spray drier to obtain a dry extract powder.

100 kg (when dried) of the extract of the dried product of Hamanilla mushroom in Example 2 was poured into 1,500 kg of warm water at 45 to 55 ° C., and 0.1 kg of the cellulase and 0.05 kg of pectinase derived from the filamentous fungus were added and stirred for 5 hours. Perform enzyme treatment.
The solution obtained by the enzyme treatment is heat-treated at 90 to 100 ° C. for 1 hour to inactivate the enzyme.
Next, the residue is subjected to solid-liquid separation by an effective wall centrifuge.
The liquid subjected to solid-liquid separation is rotated at 13,000 to 15,000 in a shear press type centrifuge to pass the liquid, and further subjected to solid-liquid separation. The separated liquid is passed through a stainless steel filter to which 5 kg of diatomaceous earth is attached to obtain a clear liquid.
The filtered liquid is concentrated under reduced pressure at a temperature of 60 ° C. or lower to make the final liquid amount 15 kg. The container is sterilized by heating at 90 ° C. for 30 minutes and filled in a hot state.

The obtained concentrated liquid was a solution which did not contain sugar alcohols such as mannitol and sorbite and from which a water-soluble high molecular weight polysaccharide containing β-glucan or the like could be extracted by about 5 to 50% of the content in dried yellow mushroom. Was.
Dextrin in the same amount as the solid content was added to the obtained concentrated liquid, and dried with a spray drier to obtain a dry extract powder.
The extract of Amanita velutipes in Example 3 is placed in a shelf dryer, and dried by heating at 40 ° C. under reduced pressure. The dried extraction residue is crushed to a certain size in a crusher. Next, the mixture is transferred to a ball mill and pulverized until it passes through a 100-mesh sieve. The dried powder has a yield of about 30 to 50% of the dried mushroom mushroom.

Claims (10)

A method for extracting mushroom components, comprising the following steps (1) to (6):
(1) a step of extracting raw, frozen or dried mushrooms in 5 to 100 parts by weight of water at 30 ° C. or lower per 1 part by weight of the mushrooms;
(2) The raw, frozen or dried mushrooms and the extraction residue in the step (1) , or the extraction residue in the step (1) are treated with 5 to 5 parts by weight of the mushrooms and / or the extraction residue. Extracting in 100 parts by weight of water at 70 ° C. or higher,
(3) converting the raw, frozen or dried mushrooms and the extraction residue in the step (1) and / or (2) or the extraction residue in the step (1) and / or (2) into the mushrooms and / or Extracting by subjecting the extract residue to enzymatic treatment with a plant tissue degrading enzyme derived from a filamentous fungus in water at 30 to 90 ° C. in an amount of 5 to 100 parts by weight based on 1 part by weight of the extraction residue;
(4) a step of separately separating the fractions obtained in steps (1) to (3) by solid-liquid separation by centrifugation and / or filtration;
(5) a step of separately concentrating the obtained clear separated liquid; and (6) a step of separately drying the obtained concentrated liquid. The method according to claim 1, wherein the plant tissue-disintegrating enzymes derived from filamentous fungi are cellulase and pectinase. The method according to claim 1 or 2 , wherein in step (1), extraction is performed by mixing with a stirrer. 3. The method according to claim 1, wherein in step (1), the mushrooms are immersed in water, sufficiently contacted with water, and allowed to stand for extraction without mixing with a stirrer. In step (1), instead of 5 to 100 parts by weight of water, stirring or leaving naturally in 5 to 100 parts by weight of 30 to 100% ethanol. The method according to claim 1 or 2 , wherein the extraction is performed. The method according to claim 1 or 2 , wherein in step (1), the surface of the mushrooms is washed away with running water, and the water is recovered and extracted. In the steps (1) to (3), in the steps (2) and (3), a fresh, frozen or dried mushroom is not added, and the steps (2) and (3) are sequentially extracted from the step (1). And separately obtaining a low molecular fraction from step (1), a low molecular and high molecular intermediate fraction from step (2), and a high molecular fraction from step (3). 3. The method according to 1 or 2 . The method according to claim 1 or 2 , wherein in step (4), filtration is performed after centrifugation. The method according to claim 1 or 2 , wherein in the solid-liquid separation by filtration in the step (4), a filter aid selected from the group consisting of diatomaceous earth, celite, perlite, and crystalline cellulose is used. In step (2) and (3), and the residue dried mushrooms to be separated, according to claim 1 or 2 wherein pulverized.